Faculty Publications
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Item Effect of Calcination Temperature and Time on Synthesis of BaO-CaO-Al2O3-SiO2 Glass(Elsevier Ltd, 2018) Bhattacharya, S.; Shashikala, H.D.Alkaline-borosilicate glass of a particular composition was prepared. 30mol%BaO-15CaO-05Al2O3-40SiO2-10B2O3 glass system mix was calcined at different temperatures, from 300°C to 400°C for varying number of hours from 0 to 7 hrs. X Ray Diffraction (XRD) and Thermo Gravimetric Analysis (TGA) studies were conducted on non calcined and calcined powders. Conversion of H3BO3to B2O3 was observed from XRD studies and increase in thermal stability was confirmed from thermal analysis study. © 2017 Elsevier Ltd.Item Green approach to synthesize multi-walled carbon nanotubes by using metal formate as catalyst precursors(2013) Rajarao, R.; Badekai Ramachandra, B.The multi-walled nanotubes (MWNTs) have been synthesized in large scale by using metal formate as catalyst precursors. The calcium carbonate is used as catalyst support, it is chosen because of its non toxic and easily soluble nature. The synthesis was carried out by chemical vapor deposition method for 15 min under optimized conditions. The products were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy and X-ray diffraction (XRD) method. The purity of the as grown products and purified products were determined by thermal analysis. The obtained yield of MWNTs was about 8300 wt% relative to the nickel catalyst. This synthesis route avoids the lengthy process of calcination and reduction for the preparation of catalysts hence this method is more economical. This economical and environmental friendly synthesis route can be used for synthesizing MWNTs in large scale. Copyright © 2013 American Scientific Publishers All rights reserved.Item Structural characterization of nano-crystalline Co3O4 ultra-fine fibers obtained by sol-gel electrospinning(2013) George, G.; Anandhan, S.In this paper, we report the obtention of ultrafine fibers of cobalt oxide (Co3O4) by combining electrospinning method with high-temperature calcinations from the precursor sol of poly(2-ethyl-2- oxazoline) (PEtOx)/cobalt acetate tetrahydrate [Co(CH3COO) 2·4H2O] in water. The optimum electrospinning conditions for obtaining precursor composite nanofibers from PEtOx/Co(CH 3COO)2·4H2O solution in water, to produce ceramic nanofibers, were studied. The average fiber diameter of the precursor composite fibers measured by scanning electron microscopy (SEM) was approximately 200 nm. Thermogravimetric analysis of PEtOx was performed to estimate the suitable calcination temperature of the precursor fibers. SEM images of the ceramic fibers obtained after calcination revealed the shrinkage in diameter due to complete degradation of the polymer and Co(CH 3COO)2·4H2O. Fourier transform infrared spectroscopy was used to ensure the complete pyrolysis of polymer during calcinations of the composite fibers. Crystalline properties of the ceramic fibers were studied by X-ray diffraction and high resolution transmission electron microscopy. The ceramic fibers are polycrystalline with an average grain size of ?40 nm obtained at a calcination temperature of 773 K. It was observed that the grain sizes increased as the calcination temperature was increased, due to self assembly mechanism. © 2013 Springer Science+Business Media New York.Item Synthesis and characterisation of nickel oxide nanofibre webs with alcohol sensing characteristics(Royal Society of Chemistry, 2014) George, G.; Anandhan, S.In this study, nickel oxide (NiO) nanofibres were obtained by a sol-gel electrospinning process followed by calcination from an aqueous sol of poly(2-ethyl-2-oxazoline)/nickel acetate tetrahydrate. Thermogravimetric analysis was used to determine the degradation temperature of the composite fibres, so as to get nickel oxide nanofibres. X-ray photoelectron spectroscopy and X-ray diffraction studies revealed the complete elimination of the organic phase from NiO fibres during calcination. The change in grain size with calcination temperature was determined by X-ray diffraction. The defects in fibres resulted in the modification of their Raman spectra as compared with that of a single crystal. The magnetic properties of the fibres were reduced as the calcination temperature was increased; this is due to the presence of non-stoichiometric defects. As the calcination temperature was increased, the amount of defects was reduced, which induced a difference in the band gap energy of the fibres. Sensitivity of the NiO fibres towards five different alcohols was studied, and the sensitivity towards ethanol was the highest. © The Royal Society of Chemistry 2014.Item Structure-property relationship of sol-gel electrospun ZnO nanofibers developed for ammonia gas sensing(Academic Press Inc. apjcs@harcourt.com, 2014) Senthil, T.; Anandhan, S.Zinc oxide (ZnO) based nanomaterials have been used in various gas sensors due to the wide band gap (3.37. eV), large exciton binding energy and high mobility of charge carriers of ZnO. In this work, nanocrystalline ZnO nanofiber mats were synthesized through combined sol-gel electrospinning techniques followed by calcination, in which poly(styrene- co-acrylonitrile) and zinc acetate were used as the binder and precursor, respectively. Average diameter of the ZnO nanofibers decreased from 400 to 60. nm, while their grain size and crystallinity were enhanced by increasing the calcination temperature. Morphology and structure of the ZnO nanofiber mats were characterized by high resolution transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. ZnO nanofiber mats were found to be superhydrophilic (contact angle was close to 0°) by contact angle measurements. The sensitivity of these ZnO nanofibers in detecting gaseous ammonia was tested using an indigenous set up. Due to their high surface area and superhydrophility, these ZnO nanofiber mats were highly sensitive in sensing gaseous ammonia and the sensitivity of these mats increased as a function of their calcination temperatures. © 2014 Elsevier Inc.Item Morphological and structural characterisation of sol-gel electrospun Co3O4 nanofibres and their electro-catalytic behaviour(Royal Society of Chemistry, 2015) George, G.; Elias, L.; Hegde, A.C.; Anandhan, S.Evolution of hydrogen and oxygen are a crucial part of many renewable energy systems. The replacement of the essential and expensive components in such systems can reduce the capital cost and improve the effectiveness of those systems. In this study, Co3O4 nanofibres were fabricated from sol-gel assisted electrospun poly(styrene-co-acrylonitrile)/cobalt acetate tetrahydrate precursor composite fibres. The morphological and compositional features of the Co3O4 nanofibres obtained after calcination of the precursor nanofibers were studied using scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy. The results of X-ray diffraction study and Raman spectroscopy revealed that the average grain size of the fibres increased with the calcination temperature. Clear evidence of defects in the fibres was observed in ultraviolet-visible-near infrared and energy dispersive spectroscopic measurements. The electrocatalytic behaviour of Co3O4 nanofibres obtained at different calcination temperatures was studied using them for the water splitting reaction in an alkaline medium. The maximum efficiency in the hydrogen evolution reaction was achieved using the Co3O4 nanofibres obtained at the lowest calcination temperature, which had the highest surface area and the smallest grain size. © The Royal Society of Chemistry 2015.Item Solar light-driven photocatalytic degradation of Anthraquinone dye-contaminated water by engineered Ag@TiO2 core–shell nanoparticles(Bellwether Publishing, Ltd., 2015) Khanna, A.; Shetty K, V.K.Abstract: The Ag core–TiO2 shell (Ag@TiO2) nanoparticles were synthesized by one-pot synthesis method followed by calcination and characterized using X-ray diffraction and transmission electron microscopy. The Ag@TiO2 core–shell-structured nanocatalyst was evaluated for its photocatalytic activity towards the degradation of Acid Blue-129 (AB-129), an Anthraquinone dye under solar light irradiations. The nanoparticles were engineered for efficient photocatalytic degradation of AB-129 by varying the parameters such as catalyst composition, calcination temperature, and calcination time. The catalyst composition with Ag to Ti molar ratio of 1:1.7, calcination temperature of 450°C, and time of 3 h were found to be the optimum for the efficient photocatalytic degradation of AB-129. The efficacy of Ag@TiO2 was compared with commercial TiO2, synthesized nano-TiO2, and Ag-doped TiO2 for the photocatalytic degradation of AB-129 and enhanced dye degradation was obtained with Ag@TiO2. This enhanced activity of Ag@TiO2 may be attributed to the trapping of conduction band electrons in Ag core and subsequent discharge on supply of air. Solar photocatalytic degradation of AB-129 dye using Ag@TiO2 followed Langmuir–Hinshelwood kinetics. Ag@TiO2 can be exploited as an efficient catalyst for the degradation of dye and textile industry wastewater. © 2014, © 2014 Balaban Desalination Publications. All rights reserved.Item Tuning characteristics of Co3O4 nanofiber mats developed for electrochemical sensing of glucose and H2O2(Elsevier B.V., 2016) George, G.; Anandhan, S.Nano-crystalline Co3O4 nanofibrous mats were fabricated by calcining the precursor nanofibers obtained by electrospinning of a sol comprising of a unique polymeric binder poly(2-ethyl-2-oxazoline) and cobalt acetate tetrahydrate in water. The influence of the calcination temperature used for the synthesis of the oxide nanofibers from the xerogel fibers on various physico-chemical properties of the former was studied. The Co3O4 nanofibers obtained at 400 °C had the highest electrochemical sensitivity towards glucose and H2O2. Further, the results prove that Co3O4 nanofibers can be used for the detection of glucose and H2O2 concurrently as the response times taken by these moieties are different. Therefore, one can differentiate the concentration of glucose and H2O2 by analyzing the signals obtained after the respective response time and this multiple sensitivity of Co3O4 can be applied in the field of biosensors. © 2016 Elsevier B.V.Item Some new observations on the structural and phase evolution of nickel titanate nanofibers(Elsevier Ltd, 2017) Kumar, B.S.; Shanmugharaj, A.M.; Kalpathy, S.K.; Anandhan, S.In this study, we report for the first time the synthesis of nickel titanate (NTO) nanofibers containing a mixture of ilmenite and spinel phases of NTO, at an atypical low temperature. Precursor nanofibers produced by sol-gel electrospinning were calcined at three different temperatures to produce the NTO nanofibers. Thermal analysis along with X-ray photoelectron spectroscopy confirmed the formation of non-crystalline stable phases of TiN and Ti-O-N that restrained the formation of ilmenite NTO, and the Ni-rich environment pushed the Ti atoms to tetrahedral sites to form a defective spinel structure. The crystallite size of spinel NTO was observed to increase as a function of the calcination temperature above 700 °C, as the activation energy for coalescence and growth of spinel NTO was favorable. NTO nanofibers obtained above the calcination temperature of 700 °C exhibited new band gap energy around 2.5 eV in Tauc plot. Oxygen vacancies in these ceramic nanofibers decreased as the calcination temperature was increased. A hypsochromic shift of 20 nm in the photoluminescence spectra suggested that the material had a Ni2+ rich NTO (spinel). © 2017 Elsevier Ltd and Techna Group S.r.l.Item Sol–gel electrospun mesoporous ZnMn2O4 nanofibers with superior specific surface area(Springer New York LLC barbara.b.bertram@gsk.com, 2017) Shamitha, C.; Senthil, T.; Wu, L.; Kumar, B.; Anandhan, S.ZnMn2O4 has application potential in lithium ion batteries, supercapacitors, sensors, and thermistors. In this study, mesoporous spinel ZnMn2O4 nanofibers were synthesized by sol–gel assisted electrospinning combined with calcination, using poly(styrene-co-acrylonitrile) as sacrificial polymeric binder. Structural, morphological and optical properties of these ceramic nanofibers were characterized. X-ray diffraction and X-ray photoelectron spectroscopy results revealed the presence of hexagonal ZnMnO3 and MnO phases in the ZnMn2O4 nanofibers produced. Based on these observations we propose a plausible mechanism of formation of ZnMn2O4 nanofibers. The nanofibers calcined at 773 K exhibit a specific surface area of 79.5 m2 g?1, which is higher than that of the zinc manganite nanofibers synthesized hitherto by sol–gel electrospinning. Moreover, this material exhibits four bandgaps, which is believed to be the first observation in ZnMn2O4 nanofibers. © 2017, Springer Science+Business Media, LLC.