international journal of pure and applied mathematics ... · 3 pure tio 2 and degussa p25. 11 -14...

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SPECTROSCOPICAL STUDIES OF MoO3 DOPED TiO2 NANOCOMPOSITES FOR

DYE DEGRADATION

MAGESAN.P1, SVIARANJANI.A

2,

1,2Associate Professor, Department of Chemistry,

BIST, BIHER, Bharath University,Chennai-73 [email protected]

Abstract

In the present study, we report MoO3-TiO2 nanocomposite film by sol-gel and solution

cast method. The synthesized nanocomposite films were characterized by X-Ray Diffraction

(XRD), Field Emission Scanning Electron Microscopy (FESEM), Energy Dispersive X-ray

(EDX) Spectra, Diffuse Reflectance Spectroscopy (DRS), Fourier Transform Infra-Red

Spectroscopy (FT-IR) and Thermo Gravimetric-Differential Thermal Analysis (TG-DTA).

Keywords: Al2O3-TiO2, nanocomposite film, Sol-gel method, Semiconductor.

INTRODUCTION

One of the main sources for the contamination of water pollution is from the textile

industries. Because the textile dyeing industries consume large quantities of water and produces

large volume of waste water from different steps in the dyeing and finishing process[1-6]. The

worldwide dye consumption for dyeing industries are around 107 kg/year.

1 Since the dyes are

stable, recalcitrant, colorant and even potentially carcinogenic and toxic[7-11], their release into

the environment causes a major threats to the environment.2 The dye contaminated waste water

cannot be easily treated because of the natural biodegradability has become increasingly difficult

task to the improved properties of dyestuffs[12-19]. A wide range of conventional methodologies

have been used to eliminate these pollutants from the waste water but the efficiency was

limited[20-26]. The modern nanotechnologies have become popular for the fabrication of

desirable nanomaterials with large surface-to-volume ratios of unique surface properties to treat

these pollutants. Nanoparticles are the key to nanotechnology; hence in-depth study of

International Journal of Pure and Applied MathematicsVolume 119 No. 12 2018, 6389-6401ISSN: 1314-3395 (on-line version)url: http://www.ijpam.euSpecial Issue ijpam.eu

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nanomaterials is an important source for producing new principles, techniques and

methods.3From environmental standpoint[27-32], heterogeneous photocatalysis is an important

pioneering technology for application in water purification. With advent of nanotechnology,

semiconductor nanoparticles have attracted much intention due to their novel optical, electrical

and mechanical properties. Among the various semiconductor nanoparticles, nanosized titanium

dioxide (TiO2) particles are the most frequently studied in the field of solar energy conversion,

photocatalysis, transparent UV protection films and chemical sensors etc.,. It has been proved to

be one of the most suitable materials in environmental remediation process due to its powerful

oxidation strength, low cost[33-39], non-toxicity and chemical stability against photo-

corossion.4-6

However, the conventional TiO2 photocatalyst suffered an obstacle when applied in

practical applications such as effective utilization of UV/solar light, large surface area

requirement for the adsorption of pollutant, that is, adverse recombination of electron and holes.

Many efforts have been made to extend the adsorption of light from UV to visible region and to

improve the photocatalytic efficiency of TiO2.7

Enhancing the rate of photoreduction by doping a

semiconductor with metal ions can produce a photocatalyst with an improved trapping-to-

recombination rate ratio. However[40-45], when metal ions or oxides are incorporated into TiO2

by doping, the impurity energy levels formed in the band gap of TiO2 can also lead to an increase

in the rate of recombination between photogenerated electrons and holes. Photocatalytic

reactions can only occur if the trapped electron and hole are transferred to the surface of the

photocatalyst. This means that metal ions should be doped near the surface of the photocatalyst

to allow efficient charge transfer. Dopants like transition metals (Fe, Al, Ni, Cr, Co, W, V and

Zr) and metal oxides (Fe2O3, Cr2O3, CoO2, SiO2, etc.,) being used to improve its applicability.8-10

The absorption threshold of TiO2 nanopowder has been shifted from UV to visible region by

doping the visible light active material and the photocatalytic efficiencies can be higher than the

International Journal of Pure and Applied Mathematics Special Issue

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pure TiO2 and Degussa P25.11-14

As a wide band gap n-type semiconductor, Molybdenum trioxide

(MoO3) is a potential material because of its wide range of stoichiometry and interesting

behavior which includes chemical,15

structural,16

electrical and optical17

properties. With surface

modification with MoO3, the TiO2 nanoparticles become much more hydrophilic, and they can

be more stably suspended in aqueous solution and it is believed that an excellent dispersibility in

aqueous solution originates from the high hydrophilicity of MoO3.18

The addition of MoO3 to

TiO2 showed high activity for the photodegradation of molasses and the MoO3-TiO2 material has

an increased surface area compared to the pure oxides. The modified material has a reduced band

gap and can absorb more light in the near-visible region and thus accelerate the rate of

decomposition.19

In this study, we have prepared MoO3-TiO2 nanocomposite film by employing

Tween-80 (T-80) as templating agent.

2. Experimental

2.1. Materials and Methods

Titanium Tetra IsoPropoxide (TTIP) and Tween-80 were purchased from Spectrochem,

Molybdenum trioxide (MoO3) from SRL. Glacial acetic acid was obtained from Qualigens were

purchased and used as received. Freshly prepared de-ionized water was used in all the experiments.

2.2. Synthesis of MoO3-TiO2 and TiO2 nanocomposites

MoO3 nanoparticles were suspended in 20 ml of distilled ethanol and stirred for 30

minutes. To the homogeneous dispersion 3 ml of tween-80 was added under stirring and further

stirred for 30 minutes. A mixture of 3 ml TTIP with 10 ml isopropyl alcohol was added drop wise

into the suspension and the stirring was continued for 2 h to get a gel. The resultant gel was filtered

off and washed thoroughly with 1:1aqueous ethanol, filtered and then oven dried at 120 ºC for 6 hrs.

The solid sample was calcined at 500 ºC for 3 hrs using an electrical muffle furnace.


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2.3. Casting of MoO3-TiO2 nanocomposite film

1 g of prepared MoO3-TiO2 composites was added into 100 mL of 1% (v/v) acetic acid) and

sonicated for 30 minutes and stirred continuously for 12 hrs until the clear solution was obtained.

The mixture solution was cast onto the petri plates and dried at room temperature for 48 hrs to obtain

the composite film.

2.5. Characterization techniques:

The following physiochemical techniques have been used to characterize the prepared

catalysts. To characterize the phase structure of the MoO3-TiO2 nanocomposite film; a Bruker D2

Phaser Desktop X-ray Diffractometer equipped with Ni-filtered Cu Kα radiation (λ=1.542 Å) and

operated at an accelerating voltage and emission current of 30 kV and 10 mA, respectively. Data

were acquired over the range of 2θ from 0° to 70 °C with a step size of 0.0017 and a scan rate of

7°/min. Field Emission Scanning Electron Microscopy (FESEM) was performed to examine the

surface morphology of the prepared nanocomposites using DXS-10 ACKT scanning electron

microscope equipped with EXS, which was used to study the elemental composition. For Fourier

transform infrared spectroscopy (FT-IR) analysis, the KBr pellets were prepared from the Al2O3

-TiO2 nanocomposites. FT-IR analysis was performed using a spectrophotometer (Perkin

Elmer RX1 instrument). Thermogravimetric-differential thermal analysis (TG-DTA) of the

nanocomposites was taken on WATERS SDT Q 600 TA model instrument. Mechanical properties

(Tensile strength and Elongation) of the films were determined according to ASTM standard method

with Universal Testing Machine (TNUM-5900). The film was cut into (7x3 cm) rectangular shapes

and measured.

3. Results and Discussion


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3.1. Surface morphology of MoO3-TiO2 nanocomposite film

Field Emission Scanning Electron Microscopy (FESEM) was used to investigate the surface

morphology of the prepared MoO3-TiO2 composite film. The FESEM pictures of MoO3-TiO2

nanocomposite film are shown in the Figure. The MoO3-TiO2 nanocomposite film has aggregated

particle structure with almost spherical morphology. But at the same time, it reveals the

agglomeration of the nanoparticles which may be due to the presence of templating agent.

3.2. Elemental composition

The elemental compositions of the MoO3-TiO2 nanocomposite film were studied by Energy

Dispersive Analysis of X-rays (EDAX). Figure 2 depicts the EDAX analysis of the MoO3-TiO2

composite film from a selected areain the binding region of 0-10 keV. The signals from the spectra

reveal the presence of Ti, O, Al and C in the prepared nanocomposites. The result corroborates the

formation of MoO3-TiO2 nanocomposite film.


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3.3. Crystalline phases

The crystalline phases of the prepared MoO3-TiO2 nanocomposite film were studied by X-

Ray Diffraction analysis. Figure 4 depicts the XRD pattern of the prepared nanocomposites. In

MoO3-TiO2 composite film, TiO2 exists in anatase phase show their sharp characteristic peaks at 2θ=

25.3°, 37.8°, 48.1°, 54.0°, 55.1°, 62.8° and 75.0° corresponds to the (101), (004), (200), (105), (211),

(204) and (215) planes agree well to standard JCPDS card No. 89-4921 and hence confirms that the

nanocomposite have been predominantly crystalline in nature with anatase phase. There is no

characteristic peaks of MoO3 has been observed and hence it can be established that doping of MoO3

did not influence the crystal structure of the TiO2 particles.

3.1. Crystal Structure:


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The average crystallite sizes of the nanocomposites have been deduced from the half-

width of the full maximum (HWFM) of the 101anatase peak of TiO2 using Scherrer equation (Eq. 2),

t = K/cos, (2)

Where t is the crystallite size, K is the shape factor of value 0.9, is the wavelength of

the X-ray used. is the Bragg’s diffraction angle, is the corrected line broadening, = b - s, b is

the broadened profile width of the experimental sample and s is the standard profile width of the

reference (high purity silica) sample. Table 1 presents the average crystallite size of the prepared

nanocomposites.

3.4. Fourier Transform Infrared Spectroscopy (FTIR)

FTIR spectrum provides information on the nature of the synthesized nanocomposites. FTIR

spectra of MoO3-TiO2 nanocomposite film were presented in the figure 5. Fig. 5 also confirms the


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existence of metal oxide (TiO2) peak around 742-783 cm-1

for MoO3-TiO2 composite film. A weak

band at around 2340-2370 cm-1

may be attributed to the vibrations of atmospheric CO2.

3.5. TG-DTA Analysis

TG-DTA analysis was carried out to study the thermal decomposition behavior of the

synthesized MoO3-TiO2 nanocomposite film is shown in the figure 6. The synthesized chitosan film

shows two weight loss curves, first stage of weight loss was due to evaporation of water and the

second stage of weight loss was due to the degradation of the polymer chain. In TGA, three

noticeable steps observed, which are in the range of 200- 340 °C, 341- 400 °C and 500 - 585 °C. The

TGA curve shows two exothermic peaks and the first exothermic peak with a maximum of 282 °C,

sharp and narrow and this may be attributed to the burnout of the templating agent. The second weak

exothermic peak corresponds to the crystallization process of TiO2 with a maximum of 354 °C.26

In

TG-DTA curve of Al2O3-TiO2, two main exothermic peaks has been found, the larger peak centered

around 363 °C and sharp peak centered around 401 °C. This may be attributed to the burnout of the

surfactant template and crystallization process, respectively.


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4. Conclusions

In summary, a kind of novel MoO3-TiO2 nanocomposite film was prepared by a simple

method. The synthesized materials were characterized by XRD, FT-IR, TG-DTA and FESEM with

EDAX.

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