Materials Sciences and Applicatio ns, 2011, 2, 676-683
doi:10.4236/msa.2011.26093 Published Online June 2011 (http://www.SciRP.org/journal/msa)
Studies on Photocatalytic Degradation of Acridine
Orange and Chloroform Sensing Using as-Grown
Antimony Oxide Microstructures
Aslam Jamal*, Mohammed Muzibur Rahman, Mohammed Faisal, Sher Bahadar Khan
Centre for Advanced Materials and Nano-Engineering (CAMNE) and Department of Chemistry, Faculty of Sciences and Arts, Na-
jran University, Najran, Kingdom of Saudi Arabia.
Received December 7th, 2010; revised December 30th, 2010; accepted May 18th, 2011.
ABSTRACT
Flower shaped antimony oxide (Sb2O3) microstructures were synthesized in a large quantity via simple solution method
using aqueous mixtures of antimony chloride and hexamethylene diamine (HMDA). The morphological characteriza-
tions were done by field emission scanning electron microscopy (FESEM), which revealed that the synthesized products
possess flower-shaped microstructures. The detailed structural characterizations performed by X-ray diffraction (XRD),
Fourier transform infrared spectrophotometer (FT-IR) and Raman spectrophotometer confirmed that the synthesized
microstructures are well-crystalline antimony oxide. The Energy dispersive spectroscopy (EDS) shows that the grown
products are composed of Sb and O. Optical properties of the synthesized products were characterized by UV-Visible
spectrophotometer which exhibits a well defined peak at ~291.0 nm. The photo-catalytic activity of the Sb2O3 micro-
structures was evaluated by degradation of acridine orange (AO), which mineralized almost 63.0% in 150 min. The
chemical sensing properties of Sb2O3 microstructures was also studied by I-V technique using chloroform as a detecting
solvent. The fabricated chloroform sensor demonstrates good sensitivity of 0.1154 µA·cm–2·mM–1, lower-detection limit
(~0.1 mM), large-linear dynamic range (LDR, 0.122 mM to 1.22 M) with linearity (R = 0.7898) in short response time
(10.0 sec).
Keywords: Antimony Oxide Microstructures, XRD, FE-SEM, Photo Degradation, Acridine Orange, Chloroform
Chemical Sensing
1. Introduction
Developing nano-science and nanotechnology is getting
valuable attention in terms of research and development
at the present time. In the field of nanotechnology, the
antimony oxide nano-crystalline particles emerges as a
challenging prospect due to having amazing preparation,
characterization, catalytic degradation, and fabrication as
well as their wide range of other applications. The syn-
thesis of nano-materials has received remarkable atten-
tion in view of the size, shape, structural arrangement,
properties and potential applications in advance level.
Generally, Sb2O3 is used as conductive materials, high-
efficiency flame-retardant synergist in polymers, dyes,
pigments, paints, adhesives, and industrial coating mate-
rials [1-3]. Sb2O3 nano-rods, nano-particles, nano-tubes,
nano-belts [4-6] and hollow spheres [7] have been fabri-
cated by various conventional routes and techniques.
Micro-structured antimony oxides can be prepared by
various general methods including vapor-solid route [8],
hydrothermal synthesis [9,10], vapor condensation [10,
11], sol-gel [12], X-ray radiation–oxidization route [13],
and gas condensation [14] techniques. However, scientist
are quite interested on controlled growth, mechanism,
characteristics, and advanced applications of the Sb2O3
microstructure [15]. During the past decades, many re-
searchers have put focus on searching for a direct and
effective method to solve this problem [16,17]. Recently,
the opt-electronic and surface properties of Sb2O3 micro-
structures have been extensively studied [2,3]. Here we
further investigate their property as a photo-catalyst and
chemi-sensor.
Organic dyes such as acridine orange are the common
pollutants and affect the environment due to its hazard-
ous and carcinogenic nature. Thus detoxification of these
organic pollutants needs an urgent and effective process.

Studies on Photocatalytic Degradation of Acridine Orange and Chloroform Sensing Using 677
as-Grown Antimony Oxide Microstructures
Several methods have been used but photo-catalytic deg-
radation is one of the superlative and attractive substi-
tutes for the degradation of these organic pollutants.
Therefore, Sb2O3 has been proposed as a catalyst for the
detoxification of organic dye in the presence of UV ra-
diation.
Organic solvents are also one of the hot environmental
problems and badly effect the environment due to their
toxicity. One of these organic solvents is chloroform
which cause cardiac or respiratory arrest [18] and depress
the central nervous system [19]. Thus it is very important
organic compound to have details study and develop de-
vices or sensors for the detection and quantification of
chloroform using microstructure materials. In general,
metal oxides are being extensively utilized due to their
unique surface activities imparted by huge surface areas,
which can make them ideal sensing elements as chemi-
sensors. The detection of chloroform in liquid phase by
I-V technique using antimony oxide surface is developed
for the first time.
In the present investigation we have made an attempt
to develop a photo-catalyst and chemi-sensor and for this
purpose antimony oxide (Sb2O3) microstructures were
synthesized. Sb2O3 microstructures were characterized by
UV, FT-IR, Raman spectroscopy, XRD, FE-SEM and
EDS. These microstructures were applied for catalytic
application and sensing application and demonstrated
good degradation and sensing properties.
2. Experimental
2.1. Materials and Methods
Analytical grade antimony chloride, hexamethylene dia-
mine, ammonium hydroxide, acridine orange, and chlo-
roform were purchased from Sigma-Aldrich and used as
received. The solution was made in double distilled water
before performing any reaction. For the synthesis of an-
timony oxide microstructure, the solutions were prepared
by adding antimony chloride (0.5 M, 50.0 mL) and
hexamethylene diamine (0.5 M, 50 mL) in distill water in
equimolecular proportion. The pH (9.3) was adjusted by
adding drop wise ammonium hydroxide and then mag-
netically stirred for 6 hour at 60.0˚C. After cooling, white
precipitates were obtained and washed with acetone for
two to three times and dried at room temperature. The
as-grown microstructure antimony oxide does reveal
better photo catalytic activity and chemical sensing
property. For this purpose, photo-degradation of AO is
investigated as model dye compound that results in a
better chemical action on antimony oxide microstructure.
Chloroform was used as model compound for sensor
application. Structural characterizations of the as-grown
materials were investigated using field emission scanning
electron microscope (FE-SEM; JSM-7600F, Japan),
x-ray diffraction (XRD; X’Pert Explorer, PANalytical
diffractometer) data was executed with Cu-Kα1 radiation.
Fourier transforms infrared spectrometer (FT-IR; Perkin
Elmer) spectrum was recorded in KBr dispersion in the
range of 400 to 4000 cm–1. UV/visible spectrum were
recorded at 291 nm (Perkin Elmer-Lambda 950-UV-
visible spectrometer). Raman-scattering spectrum was
measured at room temperature with the Ar+ laser line as
an excitation source. The chemical sensing of Sb2O3
electrodes have been primarily investigated by I-V tech-
nique, where chloroform is used as a target compound. A
thin-film was fabricated on electrode substrate by Sb2O3
micro-materials with conducting binder for fabricating
the sensor substrate.
2.2. Photo-Catalytic Experiments
Photo-degradation of AO was examined by optical ab-
sorption spectroscopy. The catalytic reaction was carried
out in a 250.0 mL beaker, which contain 150.0 ml of AO
dye solution (0.03 mM) and 150.0 mg of catalyst. Prior
to irradiation, the solution was stirred and bubbled with
oxygen for at least 15 min in the dark to allow equilib-
rium of the system so that loss of compound due to the
adsorption can be taken into account. The suspension
was continuously purged with oxygen bubbling through-
out the experiment. Irradiation was carried out using
250W high pressure Mercury lamps. Samples (5.0 ml)
were collected before and at regular intervals during the
irradiation and acridine orange solution were separated
from the photo-catalyst by centrifugation before analysis.
The degradation was monitored by measuring the ab-
sorbance using UV-visible spectrophotometer (Lambda
950). The absorbance of AO (0.03 mM) was followed at
491.0 nm wavelength.
2.3. Fabrication of Gold Electrode Using Sb2O3
Gold electrode (surface area, 0.0216 cm2) is coated with
as-grown Sb2O3 using butyl carbitol acetate (BCA) and
ethyl acetate (EA) as a coating agent. Then it is kept in
the oven at 60.0˚C for 3.0 h until the film is completely
dried. 0.1 M phosphate buffer solution at pH 7.0 is made
by mixing 0.2 M Na2HPO4 and 0.2 M NaH2PO4 solution
in 100.0 mL de-ionize water.
2.4. Detection of Chloroform Using I-V
Technique
A cell is constructed consisting of microstructure coated
gold electrode as a working electrode and Pd wire is used
as counter electrode. Chloroform solution is diluted at
different concentrations in DI water and used as a target

Studies on Photocatalytic Degradation of Acridine Orange and Chloroform Sensing Using 678
as-Grown Antimony Oxide Microstructures
chemical. Amount of 0.1 M phosphate buffer solution
was kept constant as 20.0 mL for all measurement. Solu-
tion was prepared with various concentrations of chloro-
form in DI water. The ratio of voltage and current (slope
of calibration curve) is used as a measure of chloroform
sensitivity. Electrometer is used as a voltage sources for
I-V measurement in simple two electrode system.
3. Results and Discussion
3.1. UV/Visible Spectroscopy
An optical property is one of the most important proper-
ties of any material for evaluation of its photo-catalytic
activity. The wavelength (

max) of as-grown Sb2O3 was
measured by using UV/visible spectrometer and pre-
sented in Figure 1. It displays a well-defined and strong
absorption peak at 291.0 nm which is a characteristic
absorption peak corresponds to the orthorhombic type of
Sb2O3. No other peak related with impurities and struc-
tural defects were observed in the spectrum which con-
firms that the synthesized micro-materials contain only
crystalline Sb2O3. Further band gap energy was calcu-
lated on the basis of the maximum absorption band of
Sb2O3 microstructures and found to be 4.26 eV according
to Equation (1).
1240
bg
E

 (eV) (1)
where Ebg is the band-gap energy and l is the wavelength
(nm) of the photo catalyst.
3.2. FT-IR Spectroscopy
The FT-IR spectrum (Figure 2) of as-grown Sb2O3
powder was measured with standard KBr powder by
spectrometer. The absorption band at 546 cm–1 and 690
cm–1 represent the stretching frequencies (Sb-O) and ox-
ide bridge functional group (O-Sb-O) in Sb2O3 [20]. The
absorption band at 3450 cm–1 is mainly due to the
stretching vibration of H2O (O-H) on the surface hy-
droxyl group or absorbed water. The peak at 1605 cm–1 is
observed due to bending vibration of H2O. The lower
intensity of the peak revealed the low contents of mois-
ture in the as-grown sample. The peak at 1420 cm–1 was
assigned to CO2 absorbed from the environment.
3.3. Raman Spectroscopy
Raman spectroscopy was used to elucidate the structure
of the as-grown product and discriminate from other
metal oxides. Figure 3 shows the Raman spectrum taken
using Raman microscope objective at low laser power at
room conditions. The main features of the wave-number
are observed at about 220, 298, 443, 505, 590, and 685
Wave length (nm)
Figure 1. UV/visible spectrum of as-grown Sb2O3 synthe-
sized compound.
Wave number (cm
–1
)
Figure 2. FT-IR spectrum of as-grown Sb2O3 microstruc-
ture with standard KBr compound.
Figure 3. Studies of Raman spectroscopy of as-grown Sb2O3
microstructures.

Studies on Photocatalytic Degradation of Acridine Orange and Chloroform Sensing Using
as-Grown Antimony Oxide Microstructures
679
cm–1 which are responsible for Sb-O stretching vibration
[21]. These large bands may be assigned to a magnetite
phase of antimony oxide micro-flowers.
other than Sb and O were detected. The atomic percent of
Sb and O were determined in the as-grown microstruc-
ture as 42.76% and 57.24%, respectively.
3.4. XRD Analysis 4. Applications
The crystal phase of the as-grown antimony oxide was
investigated by XRD analysis and shown in Figure 4.
XRD analysis showed diffraction peaks which could be
indexed to (110), (111), (121), (131), (002), (112), (211),
(221), (002), (240), (052), (161), (113), (133), (072),
(341), and (312) phases, which revealed the existence of
well-crystalline orthorhombic type of Sb2O3. The diffrac-
tion pattern of the as-prepared sample matches JCPDS #
74-1725. The diffraction peaks showed that the antimony
oxide produced different crystalline phase [22,23]. X-ray
diffraction thus confirmed that the obtained microstruc-
ture is well-crystalline orthorhombic type of Sb2O3.
4.1. Photo-Catalytic Degradation
Figure 6(a) exhibits the change in absorption spectra for
the photo-catalytic degradation of AO dye as a function
of irradiation time. It is found that irradiation of aqueous
suspension of AO dye in the presence of Sb2O3 micro-
structure leads to decrease in absorption intensity. It can
be seen that the maximum absorbance at 491.0 nm
gradually decreases with increase in irradiation time.
Figure 6(b) shows the change in absorbance as a func-
tion of irradiation time for the dye derivative in the ab-
sence and presence of Sb2O3 microstructure. Irradiation
of an aqueous solution of AO in the presence of synthe-
sized microstructure leads to decrease in absorption in-
tensity. Figure 6(c) shows a plot for the percent degrada-
tion vs irradiation time (min) for the oxygen saturated
aqueous suspension of acridine orange (AO) in the pres-
ence and absence the synthesized metal oxide micro-
structures. It could be seen from the figure that 63.0% (in
the presence of Sb2O3 microstructure) of the compound
degraded after 150.0 minutes of irradiation time whereas
in the absence of photo-catalyst no observable loss of dye
3.5. Measurement of FE-SEM & EDS
Morphology of the microstructure was investigated by
FE-SEM and shown in Figure 5. High and low magnifi-
cation of FESEM images [Figures 5(a-c)] showed flower
shape structure in micro-level for the as-grown products.
The EDS spectrum corroborated the composition of
Sb2O3, which is presented in the Figure 5(d). The EDS
spectra indicate that the as-grown microstructure is
composed of Sb and O. No other peak related to elements
Figure 4. XRD pattern of as-grow n synthesized Sb2O3 microstructures.

Studies on Photocatalytic Degradation of Acridine Orange and Chloroform Sensing Using 680
as-Grown Antimony Oxide Microstructures
(a) (b)
(c) (d)
Figure 5. The FE-SEM morphology of as-grown Sb2O3. (a) to (c) low to high magnified images and (d) is EDS spectrum of as
grown antimony-oxide powder.
(a) (c)
Figure 6. Photo-catalytic degradation of AO using mf-Sb2O3. (a) Spectrum of AO at different time interval; (b) Comparison
of absorbance and (c) % degradation in different time intervals of AO in presence and absence of as-grown mf-Sb2O3.

Studies on Photocatalytic Degradation of Acridine Orange and Chloroform Sensing Using
as-Grown Antimony Oxide Microstructures
681
generate superoxide radical anion [24-26] as mentioned
in the Equation (1)-(3).
could be seen. Above results clearly indicate that pre-
pared microstructure showing considerable photo cata-
lytic activity has very simple synthesis procedure and
low cost, so it can also be used as a photo catalyst beside
other metal oxide.
MO
x
cb vb
heh 


 (1)
2
O
CB
e2 O



 (2)
Antimony oxide is one of the promising semiconduc-
tors due to their various morphological (micro-flower
shape) and chemical properties, availability, easy to use,
easy to synthesis, less toxic, lower cost, higher surfaces
area, and high absorption of light quanta. Mechanism of
heterogeneous photo catalysis has been discussed exten-
sively in literature. Briefly when metal oxide absorb en-
ergy which is more than its band gap energy it results in
the generation of electron and hole pairs with free elec-
trons produced in the empty conduction band (CB
e

)
leaving behind an electron vacancy or “hole” in the va-
lence band (VB h). During this photo catalytic activity, the
electron and hole may migrate to the catalyst surface
where they participate in redox reactions. Specially, h+
VB
may react with surface-bound H2O or OH– to produce the
hydroxyl radical and is picked up by oxygen to

CB
e
2
HOOH H
VB
h


 
 (3)
The hydroxyl radicals () and superoxide radical OH
anions (2 O

) are shows as a primary oxidizing species in
the photo catalytic processes and contribute to the oxida-
tion process by attacking the dye molecules and would
results in the bleaching of the AO dye.
4.2. Chloroform Detection
The as-grown flower-shape Sb2O3 was employed for the
detection of chloroform in solution phase. Pd and gold
electrodes are used as counter electrode and working
electrode respectively. I-V technique is followed to
measure the changing of current in each injection of
chemical solution in the 20.0 mL phosphate buffer solu-
(a) (b)
(c) (d)
Figure 7. I-V characterization of as-grown Sb2O3 microstructures. (a) Comparison of with and without coating surface; (b)
Comparison of with and without chloroform sample injection; (c) Concentration variation of chloroform and (d) calibration
plot.

Studies on Photocatalytic Degradation of Acridine Orange and Chloroform Sensing Using 682
as-Grown Antimony Oxide Microstructures
chloroform was used as a detecting chemical in
ons
haped Sb2O3 has been successfully
roform, the performance of the developed chloroform
nancial support to the dean-
University, Najran,
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having Sb2O3 thin film has been studied, which is pre-
sented in the Figure 7. I-V responses sensor having
Sb2O3 thin film as a function of time for the chloroform
is shown in Figures 7(a) and (b). The time delaying for
electrometer was kept 1.0 sec. The concentration of
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5. Conclusi
The micro-flower s
synthesized using SbCl3 and HMDA by direct thermal
stirrer technique in the alkaline medium. The composi-
tion and detail structural characterization have been stud-
ied by UV, FT-IR, Raman spectroscopy, XRD, FE-SEM,
and EDS which revealed that the synthesized micro-
structures are well-crystalline, possessing orthorhombic
type of Sb2O3. The potential applications on catalytic
behavior and chemical sensing were carried out with
as-grown micro-flower Sb2O3 materials. The photo cata-
lytic performance of Sb2O3 materials were evaluated by
degradation of AO which efficiently degraded the dye.
By applying to the detection and quantification of chlo-
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linear dynamic ranges, and response time.
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