ABSTRACT
In this work, the optical and structural properties of ultrasonically prepared CaF2 :Eu3+ nanoparticles have been reported. Ultrasonically prepared CaF2 :Eu3+ phosphor shows orange, red emission bands at 591 nm and 612 nm, respectively, when it is excited by 394 light-emitting diode (LED) excitation wavelengths. Further phosphor materials are well characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and transmission electron microscopy (TEM) techniques to confirm the phase purity, metal oxygen (MO) bonding and crystallites size of the materials. Here synthesized materials show a tube-like structure under 100 nm resolution and 0.1 mol% is the best doping value of the europium ion (Eu3+ ) in calcium fluoride (CaF2 ) that shows highest intensity when prepared with an ultrasound assisted method.
Subject(s)
Calcium Fluoride/chemistry , Europium/chemistry , Nanoparticles/chemistry , Ultrasonic Waves , Molecular Dynamics Simulation , Molecular Structure , Particle SizeABSTRACT
In the present work, the synthesis of ternary chitosan/zinc oxide/titanium dioxide (CTS-ZnO-TiO2) nanocomposite was carried out with the use of mechanical stirring (conventional) and ultrasound assisted method. The characterization of prepared CTS-ZnO-TiO2 adsorbent was carried out using XRD, TEM, FTIR and the results of these analysis methods proved the successful preparation of ternary nanocomposite. Crystal violet (CV) dye was used as a pollutant to observe the adsorption ability of the prepared nanocomposite and the nanocomposite prepared by ultrasonic-assisted method proved to be a better adsorbent. The CV dye adsorption was significant for CTS-ZnO-TiO2 nanocomposite synthesized with the use of ultrasound assisted method compared to that prepared by conventional method. It is due to the physical effects of the ultrasonic irradiations due to which formation of finely dispersed nanocomposite takes place than that by conventional method. For batch adsorption the effect of various operating parameters such as initial dye concentration, time, temperature and adsorbent dose has been evaluated. The obtained data were processed using isotherm models, adsorption kinetics and the thermodynamic behavior of the cationic dye adsorption was also studied. The isotherm data was correlated reasonably well by the Temkin adsorption isotherm. Pseudo-second-order kinetic model provided a better correlation for the experimental data compared to pseudo first order, Elovich model and power function kinetics model. Thermodynamic parameters for adsorption indicated that the dye adsorption was spontaneous and endothermic in nature.
ABSTRACT
The present work deals with the preparation of graphene oxide (GO) using Hummers-Offeman method in the presence of ultrasonic irradiations. Further loading of TiO2 photocatalyst on prepared GO was accomplished which is basically oxidation reduction reaction between graphene oxide and titanium isopropoxide that leads to the formation of graphene-TiO2 nanocomposite. Graphene-Ce-TiO2 and Graphene-Fe-TiO2 nanocomposites were prepared using one step in-situ ultrasound assisted method using GO, titanium isopropoxide, cerium nitrate, ferric nitrate, and 2-propanol. The successfully prepared graphene-TiO2, Graphene-Ce-TiO2, Graphene-Fe-TiO2 nanocomposites were then characterized using XRD, SEM and TEM analysis. The obtained XRD patterns clearly indicates the formation of anatase TiO2 on graphene nanosheets and it also indicates the presence of Ce and Fe in the Graphene-Ce-TiO2 and Graphene-Fe-TiO2 nanocomposite respectively. Further the use of the prepared nanocomposites as a photocatalyst have been studied for the degradation of crystal violet dye. The effect of various parameters such as catalyst doping, catalyst loading and initial concentration of dye on its degradation were studied. The effectiveness of the prepared catalysts were compared for the degradation of crystal violet dye. It has been observed that Graphene-Fe-TiO2 exhibits maximum photocatalytic activity compared to Graphene-Ce-TiO2 and Graphene-TiO2 nanocomposite photocatalyst.
ABSTRACT
The present work establishes in depth study of ultrasound assisted preparation of performic acid (PFA) in a continuous flow microstructured reactor. The influence of various parameters viz. formic acid: hydrogen peroxide molar ratio, flow rate, temperature and catalyst loading on the PFA formation were studied in a continuous flow microstructured reactor. In a continuous microstructured reactor in the presence of ultrasonic irradiation, the formation of PFA was found to be dependent on the molar ratio of formic acid: hydrogen peroxide, flow rate of reactants, temperature and catalyst loading (Amberlite IR-120H). The optimized parameter values are 1:1M ratio, 50mL/h, 40°C and 471mg/cm3 respectively. Further, the performance of Amberlite IR-120H catalyst was evaluated for three successive cycles in continuous microstructured reactor. The performance of catalyst was found to be decreased with the usage of the catalyst and is attributed to neutralization of the sulfonic acid groups, catalyst shrinkage, or loss in pore sites. The experimental results revealed that, for an ultrasound assisted synthesis of PFA in continuous microstructured reactor the observed reaction time was even less than 10min. The observed intensification in the PFA synthesis process can be attributed to the intense collapse of the cavities formed at low temperature during ultrasonic irradiations, which further improved the heat and mass transfer rates with the formation of H2O2 during the reaction. The combined use of ultrasound and a continuous flow microstructured reactor has proved beneficial process of performic acid synthesis.
ABSTRACT
The present work reports on an efficient and simple one pot synthetic approach for aluminium nanoflakes and nanoparticles based on the intensification using ultrasound and provides a comparison with the conventional approach to establish the cutting edge process benefits. In situ passivation of aluminium particles with oleic acid was used as the method of synthesis in both the conventional and ultrasound assisted approaches. The aluminium nanoflakes prepared using the ultrasound assisted approach were subsequently dispersed in di-octyl adipate (DOA) and it was demonstrated that a stable dispersion of aluminium nanoflakes into di-octyl adipate (DOA) is achieved. The morphology of the synthesized material was established using the transmission electron microscopy (TEM) analysis and energy dispersive X-ray analysis (EDX) and the obtained results confirmed the metal state and nano size range of the obtained aluminium nanoflakes and particles. The stability of the aluminium nanoflakes obtained using ultrasound assisted approach and nanoparticles using conventional approach were characterized using the zeta potential analysis and the obtained values were in the range of -50 to +50mV and -100 to +30mV respectively. The obtained samples from both the approaches were also characterized using X-ray diffraction (XRD) and particle size analysis (PSA) to establish the crystallite size and particle distribution. It was observed that the particle size of the aluminium nanoflakes obtained using ultrasound assisted approach was in the range of 7-11nm whereas the size of aluminium nanoparticles obtained using conventional approach was much higher in the range of 1000-3000nm. Overall it was demonstrated that the aluminium nanoflakes obtained using the ultrasound assisted approach showed excellent morphological characteristics and dispersion stability in DOA showing promise for the high energy applications.
ABSTRACT
A novel continuous process for the synthesis of calcium carbonate based on precipitation reaction has been developed involving the sequential operation of two sonochemical reactors for the first time. The reactors were also operated as control (conventional approach without ultrasound) to clearly establish the process intensification benefits due to the use of ultrasound. The effect of different operating parameters such as Ca(OH)2 concentration, CO2 flow rate and Ca(OH)2 slurry flow rate on the particle size has been investigated. The obtained calcite particles were characterized using Fourier transform infrared (FTIR), wide angle X-ray diffraction (XRD) and particle size distribution (PSD) analysis. The morphology of the obtained particles was also analyzed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). It was established that the average particle size obtained in the presence of ultrasound was smaller with much narrow size distribution as compared to the conventional approach. Further, the average particle size was established to decrease with an increase in the Ca(OH)2 slurry concentration and CO2 flow rate with the optimum conditions giving a particle size of 164nm. The particle size was also influenced by the Ca(OH)2 slurry flow rate and under optimum condition of Ca(OH)2 slurry flow rate as 24mL/min, particle size of 135nm was obtained. Only calcite phase of CaCO3 was observed to be formed as established based on the XRD analysis during both the synthesis approaches confirming the stability of the obtained particles. It was also observed that the shape of the crystals varied with the method of synthesis. Rhombohedral calcite particles were formed in the presence of ultrasound whereas the conventional stirring method resulted in spindle shaped particles. Overall, the utility of the ultrasound assisted approach has been clearly established with novel results based on the use of sonochemical reactors in series.
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In this article, an acoustic cavitation engineered novel approach for the synthesis of TiO2, cerium and Fe doped TiO2 nanophotocatalysts is reported. The prepared TiO2, cerium and Fe doped TiO2 nanophotocatalysts were characterized by XRD and TEM analysis to evaluate its structure and morphology. Photo catalytic performance of undoped TiO2 catalyst was investigated for the decolorization of crystal violet dye in aqueous solution at pH of 6.5 in the presence of hydro dynamic cavitation. Effect of catalyst doping with Fe and Ce was also studied for the decolorization of crystal violet dye. The results shows that, 0.8% of Fe-doped TiO2 exhibits maximum photocatalytic activity in the decolorization study of crystal violet dye due to the presence of Fe in the TiO2 and it may acts as a fenton reagent. Kinetic studies have also been reported for the hybrid AOP (HAOP) that followed the pseudo first-order reaction kinetics.
ABSTRACT
In the present work, sodium zinc molybdate (SZM) nanoparticles were prepared using conventional and an innovative ultrasound assisted co-precipitation of sodium molybdate, zinc oxide and HNO3 at different temperatures. Prepared product was characterized by XRD, TEM, FT-IR, particle size distribution (PSD), TGA and DTA techniques. TEM analysis shows the spindle-shaped morphology of the formed SZM nanoparticles. The average particle size of SZM nanoparticles is found to be lower in case of sonochemical method (78.3 nm) compared to conventional method (340.2 nm) which is attributed to faster solute transfer rate due to ultrasonic irradiation leading to rapid nucleation and restricted growth of SZM nanoparticles. Further, the kinetics of synthesis of SZM nanoparticles are studied using the sonochemical method at different operating temperature and conventional method at 80°C. It is shown that the rate of reaction is significantly faster at 40°C compared to other temperatures and also conventional method. This can be attributed to intense cavity collapse at lower temperature (low vapour pressure) compared to higher temperature (high vapour pressure) of the reaction mixture.
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Ultrasound assisted in-situ semi-batch emulsion polymerization has been used for the preparation of polyaniline (PANI) and PANI/ZnMoO4 nanocomposite with different loading of ZnMoO4 (ZM) nanoparticles. ZM nanoparticles were functionalized using Myristic acid (MA) for better compatibility with PANI. The cavitational effects induced due to ultrasonic irradiations have been shown significant enhancement in the dispersion of functionalized ZM nanoparticles into the PANI during ultrasound assisted in-situ emulsion polymerization process. TEM images of PANI/ZM nanocomposite particles give the direct evidence of fine dispersion and encapsulation of MA treated ZM nanoparticles in PANI matrix. The presence of ZM nanoparticles in PANI/ZM nanocomposite shows significant improvement in the mechanical (cross-cut adhesion), thermal, anticorrosion and sensing properties of PANI/ZM nanocomposite/alkyd coatings over PANI/alkyd and neat alkyd resin coating. Fine and uniform dispersion of ZM nanoparticles in PANI matrix using this novel synthesis method (PANI (p-type)/ZM (n-type) hetero-junction) improves LPG sensing ability and minimizes response time to sense LPG significantly compared with neat PANI.
ABSTRACT
Ultrasound assisted synthesis of yellow rare earth cerium zinc molybdate anticorrosion nanopigment is presented. This new class of pigment is eco-friendly alternatives to lead, cadmium and chromium pigment as these pigments contains carcinogenic species like Cr(6+) which is responsible for human disease. The synthesis of nanosized cerium zinc molybdate was carried out using cerium nitrate, sodium zinc molybdate as a precursor materials by conventional and ultrasound assisted chemical precipitation method without addition of emulsification agent. XRD, FTIR and elemental analysis confirm the formation of cerium zinc molybdate nanoparticles. The conductivity results indicate that conventional synthesis takes longer time, while in sonochemical technique (US), reaction completes within short period of time. Improved solute transfer rate, rapid nucleation, and formation of large number of nuclei are attributed to presence of cavitation. Saturation of the Ce(3+) ions reaches earlier in case of sonochemical technique which restricts the growth of particles hence smaller size is obtained. The crystallite size of cerium zinc molybdate was found to be 27nm from XRD analysis.
ABSTRACT
In this work semibatch miniemulsion was carried out wherein the effect of free radicals produced by ultrasound and an external addition of initiator was examined. Influence of different variables on polymerization rate and polymer particle size has also been investigated. Over a range of 0-4% (by wt) initiator, the polymerization rate was found to increase over a range of 0.56-1.33 g L(-1) min(-1). Similarly monomer concentration range (7.2-15 wt.%) changed the polymerization rate from 1.33 to 2.61 g L(-1) min(-1). Under optimum parametric conditions polymer particle size 50 nm were obtained with a narrow size distribution. Syndiotactic phase of PMMA was observed by controlling the formulation recipe. Although, number of reports could be found in the literature [9,13,17,18,20,22] related to batch emulsion polymerization, this experimental data could be useful for the production of large scale monodispersed PMMA latex as all of the scale-up and design parameters have been qualitatively addressed.
