S YNTHESIS AND CHARACTERIZATION STUDIES OF IRON … · materi als for different application [1-7]s....
Transcript of S YNTHESIS AND CHARACTERIZATION STUDIES OF IRON … · materi als for different application [1-7]s....
SYNTHESIS AND CHARACTERIZATION STUDIES OF IRON MOLYBDENUM
MIXED METAL OXIDE (FE2(MOO4)3) NANO – PHOTOCATALYSTS
K.Seevakan
1, S.Bharanidharan
2
Assistant Professor 1 2
Department of Physics, BIST, BIHER, Bharath University, Chennai.
Abstract
Iron molybdate Fe2(MoO4)3 nano-photocatalyst was synthesized by simplistic one-pot
microwave combustion method using urea as fuel. The formation of crystalline orthorhombic
phase of Fe2(MoO4)3 was confirmed by powder X-ray diffraction (XRD) and the functional
group was confirmed by Fourier transform infrared (FT-IR). The morphology of the sample
consists of particle-like spherical shaped nanostructures, which was confirmed by high-
resolution scanning electron microscope (HR-SEM) with energy dispersive X-ray (EDX)
analysis and high-resolution transmission electron microscope (HR-TEM) analysis. . The
present study leads to enhance the photocatalytic (PC) activity of Fe2(MoO4)3 sample after TiO2
catalyst was added. The Fe2(MoO4)3 nanoparticles (NPs) sensitized TiO2 catalyst showed
enhanced photocatalytic degradation (PCD) of methylene blue (MB) under visible light
irradiation. The alteration of Fe2(MoO4)3-TiO2 nano-composites catalyst shows higher
adsorption with synergistic effect and enhanced towards the PCD of MB dye.
International Journal of Pure and Applied MathematicsVolume 119 No. 12 2018, 5797-5811ISSN: 1314-3395 (on-line version)url: http://www.ijpam.euSpecial Issue ijpam.eu
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1. Introduction
Nano-structured magnetic materials have attracted considerable attention due to their
unusual physical and chemical properties than that of their same bulk materials. In recent years,
transition metal oxides have attracted a much interest of research in nano technology as potential
materials for different application[1-7]s. As a family of important functional magnetic materials,
metal molybdates have been widely used in photoluminescence, microwave applications, optical
fibers, scintillator materials, humidity sensors and electro-catalysis [8-17]. The molybdates
constitute an interesting group owing to their structural electronic and catalytic properties [18-
24]. Among the many metal molybdates, iron molybdate (Fe2(MoO4)3) is a particularly efficient
catalyst for the oxidation of methanol into formaldehyde and exhibits very interesting magnetic
properties [9, 10]. Iron molybdate has important industrial application as a catalyst [25-31].
Several synthesis methods were proposed for the production of iron molybdate, including
microwave synthesis [12], precipitation [13], solvothermal [14] and hydrothermal methods [15],
etc. However, the above synthesis methods require long reaction times, and involve the use of
solution, making more costly as several steps are necessary including filtration and calcinations,
etc. The synthesis methods are expensive and more difficult to apply in an industrial application.
Among the above methods microwave combustion method have many advantages, such as high
purity product, high reaction rate and energy saving. Also, this method is very simple and low
cost technique for the preparation of functional materials in nanometer range [32-36].
Nowadays metal oxides have been used as catalysts for the degradation of organic
pollutants. Among them, magnetic iron oxides are highly used, because it can be easily removed
by external magnetic field and reused several times without any change of catalytic activity.
Manikandan et al. [17-21] reported spinel ferrites prepared by microwave combustion method
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and are used as a photo-catalyst for the degradation of 4-chlorophenol (4-CP). Also, they
reported metal doped spinel ferrites for the catalytic oxidation of benzyl alcohol into
benzaldehyde [37-43]. Ding et al. [28] designed a template-free hydrothermal process to
selectively prepare monoclinic and orthorhombic Fe2(MoO4)3 micro-sized particles. Hassani et
al. [2] reported Fe2(MoO4)3 NPs in the reduction of nitrophenol isomers into their corresponding
aminophenol isomers. Hankare et al. [44-50] reported ZnFe2O4, TiO2-ZnFe2O4, TiO2-Al2O3-
ZnFe2O4 photo-catalysts for the degradation of methyl red and thymol blue. Routray et al. [30]
reported Fe2(MoO4)3 for the selective oxidation of methanol into formaldehyde. Zhang et al. [31]
reported magnetic and photocatalytic properties of Fe2(MoO4)3 microstructures by microwave-
assisted hydrothermal synthesis. Singh et al. [32] reported Fe2(MoO4)3 electro-catalysts prepared
by co-precipitation method for oxygen evolution reaction in alkaline solutions. Xu et al. [33]
reported visible-light-active TiO2 -ZnFe2O4 photo-catalyst. .
2. Experimental
2.1. Materials and synthesis procedure
All the chemicals used in this study were of analytical grade obtained from Merck, India
and were used as received without further purification. Iron nitrate (Fe(NO3)2·9H2O, 98%),
ammonium heptamolybdate (NH4)6Mo7O24·4H2O and urea ( CO (NH2)2) as the fuel are used for
this method. In case of Fe2(MoO4)3, the precursor mixture in urea was in a domestic microwave
oven and exposed to the microwave energy in a 2.45 GHz multimode cavity at 850 W for 10
minutes. Initially, the precursor mixture boiled and underwent evaporation followed by the
decomposition with the evolution of gases. When the solution reached the point of spontaneous
combustion, it vaporized and instantly became a solid. The obtained solid powders were washed
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well with ethanol and dried at 80ºC for 1h, and labeled as Fe2(MoO4)3 and then used for further
characterizations. The entire microwave combustion process produce Fe2(MoO4)3 powders in a
microwave-oven operated at a power of 850 W has produced Fe2(MoO4)3 within 10 min.
2.2. Characterization techniques
The characterization of the obtained Fe2(MoO4)3 powder were conducted by using
various techniques to verify the phase formation, crystallite size, distribution and to explore other
parameters of interest. The structural characterization of Fe2(MoO4)3 nanoparticles were
performed using Rigaku Ultima X-ray diffractometer equipped with Cu-Kα radiation (λ =1.5418
Å). The surface functional groups were analyzed by Perkin Elmer FT-IR spectrometer.
Morphological studies and energy dispersive X-ray analysis (EDX) of Fe2(MoO4)3 NPs have
been performed with a Jeol JSM6360 high resolution scanning electron microscopy (HR-SEM)..
2.3. Photocatalytic reactor setup and degradation procedure
Photocatalytic degradation (PCD) experiments were carried out in a self-designed
photocatalytic reactor. The cylindrical photocatalytic reactor tube was made up of
quartz/borosilicate with a dimension of 36 cm height and 1.6 cm diameter. The top portion of the
reactor tube has ports for sampling, gas purging and gas outlet. The aqueous methylene blue
(MB) solution containing appropriate quantity of Fe2(MoO4)3 nano photo-catalysts was taken in
the quartz/borosilicate tube and subjected to aeration for thorough mixing and placed inside the
reactor setup. The lamp housing has low pressure mercury lamps (8 x 8 W) emitting either 254
or 365 nm with polished anodized aluminum reflectors and black cover to prevent UV leakage.
Prior to photocatalytic experiments, the adsorption of MB on Fe2(MoO4)3 and TiO2 nano photo-
catalyst was carried out by mixing 100 ml of aqueous solution of MB with fixed weight of the
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respective photo-catalyst. This slurry was equilibrated for 30 minutes in a magnetic stirrer. The
PCD was carried out by mixing 100 ml of aqueous MB solution and fixed weight of nano photo-
catalysts. PCD of MB was also carried out with Fe2(MoO4)3-TiO2 mixed oxides.
3. Results and Discussion
3.1 Structural analysis
The structural and phase analysis of the samples were characterized by powder X-ray
diffraction (XRD) pattern and is shown in Figure 1. All the diffraction peaks could be indexed
to monoclinic Fe2(MoO4)3 structure, which is in good agreement with the literature values
(JCPDS file Card No. 35-0183) [31]. No other impurity peak was detected. The very high peak
intensity suggests that the material is highly crystalline. This indicates the complete
transformation of the precursor into Fe2(MoO4)3 phase. The average crystallite size of
Fe2(MoO4)3 sample was calculated using Debye Scherrer formula
cos
89.0L
3.2 FT-IR spectral analysis
Figure 2 shows the FT-IR spectra of Fe2(MoO4)3 powders. FT-IR spectra contain a broad
band between ~ 3200 and ~ 3400 cm-1
due to the O-H stretching mode [1]. Furthermore bands
related to C=O and C-O stretching modes that appear at ~1723 and ~1042 cm-1
respectively, due
to the ester groups formed [32]. The spectra of Fe2(MoO4)3 powders shows absorption bands
between ~1000 and 1120 cm-1
is mainly due to Mo=O stretching vibration. A peak at 827 cm-1
is
attributed to Mo(VI)-O tetrahedral stretching and peak at 656 cm-1
corresponds to Fe(III)-O
octahedral stretching vibration.
The sharpness of these bands is correlated to the high degree of
crystallinity of the Fe2(MoO4)3 phase.
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3.3. High resolution- scanning electron microscopy (HR-SEM) studies
The nanostructure and surface morphology of the as-prepared Fe2(MoO4)3 sample was
examined by high resolution scanning electron microscope (HR-SEM) analysis. Figure 3 shows
the HR-SEM images of Fe2(MoO4)3 samples, which clearly shows the spherical-like structure
consisting of agglomerated particles. The agglomeration of the particles with nanoparticles
structure may be due to the magnetic nature of the samples. In this microwave combustion
method the crystal formation is due to the stable nuclei via ion-by-ion addition and unit
replication. The formation of rods-like structure may be due the agglomeration and attachment
of the nano-crystals. Also, the layer-by-layer self-assembled nano-particles, which lead to the
formation of spherical-like Fe2(MoO4)3 nanostructure.
3.4. High resolution transition electron microscopy (HR-TEM) studies
To provide a further evidence for the formation of spherical-like nanoparticle
morphology of Fe2(MoO4)3 samples, high-resolution transmission electron microscopy (HR-
TEM) analysis was carried out and is shown in Fig. 4. Figure 4a shows the HR-TEM image of
Fe2(MoO4)3 spherical- like NPs with diameter ranging from 15-25 nm. It is obvious that the
spherical-like NPs are uniform in size, which is consistent with the average crystallite size
obtained from the peak broadening in XRD analysis. The Fig. 4b, shows the selected area
electron diffraction pattern (SAED) of spinel Fe2(MoO4)3, which implies that the as-prepared
samples are single crystalline in nature. SAED results show spotty ring characteristic of small
crystallites of Fe2(MoO4)3 nanoparticle without any additional diffraction spots.
3.5 Photocatalytic properties
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TiO2 supported Fe2(MoO4)3 NPs on the PCD efficiency is evaluated as shown in Figure 5.
The PCD efficiency of Fe2(MoO4)3 is very low when compared with TiO2. The PCD efficiency
of TiO2 supported Fe2(MoO4)3 (i.e. Fe2(MoO4)3-TiO2 NCs) is higher than pure Fe2(MoO4)3 NPs.
The photocatalytic activity of single phase Fe2(MoO4)3 is enhanced, when it is coupled with TiO2
to form a composite catalyst. Though, the band gap of Fe2(MoO4)3 is smaller than that of TiO2
and it is a visible light active catalyst, it exhibits lower photo-catalytic activity, due to its lower
valence band potential compared to TiO2 When TiO2 and Fe2(MoO4)3 are coupled and irradiated
with UV-Vis light, the photocatalytic activity is improved, though the charge carriers can
migrate to Fe2(MoO4)3, due to the higher VB potential of TiO2. Photocatalytic degradation was
occurred by hydroxyl radicals attack the MB.
4. Conclusions
Fe2(MoO4)3 nanoparticles were successfully synthesized by a simple micro wave
combustion method using urea as the fuel. Powder XRD results confirmed that the pure single
phase crystalline with monoclinic structure of Fe2(MoO4)3 nanoparticles. HR-SEM images show
that the morphology of the sample consists with well defined nanoparticles (NPs) structure with
agglomeration. VSM results showed ferromagnetic behavior. The PCD efficiency of Fe2(MoO4)3
is very lower than TiO2 catalyst. The PCD efficiency of TiO2 supported Fe2(MoO4)3 (i.e.
Fe2(MoO4)3-TiO2 NCs) is higher than pure Fe2(MoO4)3 NPs. These results indicated that the
Fe2(MoO4)3 nano-structures may find applications in water pollution control. Compared to other
synthetic methods, microwave combustion method is a facile, low-cost pathway for the
preparation of Fe2(MoO4)3 nano-structures.
Figure captions
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Figure 1. XRD patterns of Fe2(MoO4)3 NPs.
Figure 2. FT-IR spectra of Fe2(MoO4)3 NPs.
Figure 3. HR-SEM images of Fe2(MoO4)3 NPs.
Figure 4. HR-TEM images of Fe2(MoO4)3 NPs.
Figure 5. PCD efficiency of TiO2-supported Fe2(MoO4)3 photocatalyst (Experimental conditions:
MB = 100 mg/L, Photocatalyst = 30 mg/100 mL, k = 365 nm).
Figure captions
Figure 1. Powder XRD pattern of Fe2(MoO4)3 NPs.
10 20 30 40 50
Inte
nsi
ty (
a.u
)
2 Theta (degree)
(237
) (012
)
(11
2)
(120
) (1
20
) (- 214)
(- 144)
(220
) (212
) (1
22
)
(- 105)
(- 224
) (4
00
) (- 503)
(222
) (0
24
) (0
32
) (- 116)
(- 234)
(- 525)
(- 616)
(511
) (106
) (4
03
) (035
)
(225
)
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4000 3600 3200 2800 2400 2000 1600 1200 800
Inte
nsi
ty (
a.u
)
Wavenumber (cm-1
)
Figure 2. FT-IR spectra of Fe2(MoO4)3 NPs.
Figure 3. HR-SEM images of Fe2(MoO4)3 NPs.
a b
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0 50 100 150 200 250 300
0
20
40
60
80
100
PC
D e
ffic
ien
cy
(%
)
Time (minutes)
Photolysis
Fe2(MoO4)3
TiO2
Fe2(MoO4)3-TiO2
Figure 4. HR-TEM image (a) and SAED pattern (b) of Fe2(MoO4)3 NP
Figure 5. PCD efficiency of TiO2-supported Fe2(MoO4)3 photocatalyst (Experimental
conditions: MB = 100 mg/L, Photocatalyst = 30 mg/100 mL, k = 365 nm).
a b
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