Faculty Publications
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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 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.Item Sol-gel electrospun ZnMn2O4 nanofibers as bifunctional electrocatalysts for hydrogen and oxygen evolution reactions(Institute of Physics Publishing helen.craven@iop.org, 2019) Shamitha, C.; Shetty, A.R.; Hegde, A.C.; Anandhan, S.Electrochemical water-splitting has gained significant attention for the development of next generation fuels. The present work is an investigation on the electrocatalytic activity towards both Oxygen Evolution Reaction (OER) and Hydrogen Evolution Reaction (HER) of ZnMn2O4 (ZMO) nanofabrics synthesized by sol-gel electrospinning followed by calcination (at 500, 600 and 700 °C). Poly(styrene-co-acrylonitrile) was used as the polymeric binder for the production of nanofabrics. The morphological features of ZMO nanofabrics were studied by scanning electron microscopy and field emission scanning electron microscopy. The electrocatalytic behavior of ZMO nanofabrics obtained at different calcination temperatures was evaluated using chrono-potentiometry, cyclic voltammetry, and linear sweep voltammetry in an alkaline medium (1 M KOH). The ZMO nanofabrics calcined at 500 °C exhibited the maximum electrocatalytic activity towards HER. This can be ascribed to their superior specific surface area (79.5 m2 g-1). The nanofabrics calcined at 700 °C displayed the least potential for O2 evolution and hence they are considered to be effective for OER. The results prove that ZMO nanofabrics are promising candidates as bifunctional electrocatalysts for water-splitting applications. © 2019 IOP Publishing Ltd.Item Graphene nanoclusters embedded nickel cobaltite nanofibers as multifunctional electrocatalyst for glucose sensing and water-splitting applications(Elsevier Ltd, 2019) Kumar, B.S.; Gudla, V.C.; Ambat, R.; Kalpathy, S.K.; Anandhan, S.Nickel cobaltite (NCO) attains the apex of Sabatier-type volcano plot for electrochemical reaction compared to simple oxides due to synergetic effect of mixed transition metal cations. The combination of high surface area, aspect ratio, and porosity of electrospun NCO nanofibers (NCO-NF) enhance their electrocatalytic performance by improved electron mobility and more active sites. In the present study, NCO-NF fabricated using poly (styrene-co-acrylonitrile) (SAN) as a sacrificial polymer, were embellished with graphene nanoclusters (GNC), which augment the electrocatalytic performance of the NCO-NF. The in situ formed GNC along the NCO-NF are result of the interaction between the polar functional groups of the polymer, and the cations of precursor salts during the calcination of precursor nanofibers. The GNC/NCO-NF with least crystallite size and high aspect ratio having porous NCO nanoparticles and in situ grown GNC were developed using sol-gel electrospinning process assisted by calcination of precursor nanofibers. This simple, eco-friendly, and economical synthesis route with unique structure chemistry of SAN to form GNC and the presence of dual cations (Ni and Co) provides enhanced performance and multifunctionality to GNC/NCO-NF electrodes for electrocatalytic applications, such as biosensors and water-splitting. In the present study, the modified electrodes (GNC/NCO-NF/graphite electrode) exhibited excellent non-enzymatic glucose detection over a wide range of concentration with a lower limit of 1.2 ?M and sensitivity of 1827.5 ?A mM?1 mg?1 in 0.1 M NaOH. Further, the modified electrodes were also tuned for H2O2 detection to aid enzymatic glucose sensing. When examined for bifunctional water-splitting in 1 M NaOH, the electrode reached an onset potential of ?0.537 V and 0.735 V against reversible hydrogen reference electrode and a Tafel slope of 37.6 mV·dec?1 and 67.0 mV·dec?1 for hydrogen and oxygen evolution reactions, respectively. The results prove that GNC/NCO-NF are promising candidates as multifunctional electrocatalyst. © 2019 Elsevier Ltd and Techna Group S.r.l.