Faculty Publications
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Item Pyrolysis-controlled synthesis and magnetic properties of sol–gel electrospun nickel cobaltite nanostructures(Springer New York LLC barbara.b.bertram@gsk.com, 2018) Kumar, B.S.; Dhanasekhar, C.; Adyam, A.; Kalpathy, S.K.; Anandhan, S.Nickel cobaltite (NCO) is a binary transition-metal oxide, which is extensively used as an electrocatalyst and magnetic material. NCO nanofibers and NCO/graphene composite exhibit high electrochemical reactivity due to the directional bridging of NCO particles. This makes NCO a promising candidate electrode material for use in supercapacitors and batteries. Besides, NCO is also a promising magnetic material due to its unique structural composition, where the cations are seated in octahedral sites surrounded by oxygen vacancies. In the present work, a simple and reliable method was discovered for tuning the morphological and structural changes of nickel cobaltite (NCO) nanoparticles, which were reshaped along the NCO nanofibers, by controlling the pyrolysis soaking time. As the pyrolysis soaking time increases, NCO transforms from inverse spinel to normal spinel; and the morphology of NCO nanoparticles changes from spherical to rod-like. These changes were validated by the hypsochromic peak shifts in Raman, and FTIR spectroscopies. The magnetic measurements reveal changes in the shape of the hysteresis loop, which are explained on the basis of structural and morphological changes in the nanostructure. The net magnetisation increases and coercivity decreases, with an increase in pyrolysis soaking time. These changes in magnetic parameters are attributed to structural changes caused by the formation of oxygen vacancies, and surface effects due to switching in morphology of the NCO nanoparticle. [Figure not available: see fulltext.]. © 2018, Springer Science+Business Media, LLC, part of Springer Nature.Item Polymorph nickel titanate nanofibers as bifunctional electrocatalysts towards hydrogen and oxygen evolution reactions(Royal Society of Chemistry, 2019) Kumar, B.; Tarafder, K.; Shetty, A.R.; Hegde, A.C.; Gudla, V.C.; Ambat, R.; Kalpathy, S.K.; Anandhan, S.Producing pure H2 and O2 to sustain the renewable energy sources with minimal environmental damage is a key objective of photo/electrochemical water-splitting research. Metallic Ni-based electrocatalysts are expensive and eco-hazardous. This has rendered the replacement or reduction of Ni content in Ni-based electrocatalysts a decisive criterion in the development of bifunctional electrocatalytic materials. In the current study, spinel/ilmenite composite nickel titanate (NTO) nanofibers were synthesised using sol-gel assisted electrospinning followed by pyrolysis at different soaking temperatures (viz., 773, 973, and 1173 K). The presence of a defective spinel NTO phase (SNTO) distributed uniformly along the nanofibers was confirmed by X-ray photoelectron and Raman spectroscopy. The electron micrographs revealed the morphological change of NTO nanofibers from a mosaic to bamboo structure with an increase in pyrolysis soaking temperature. The electrocatalytic activity of NTO nanofibers obtained at different pyrolysis soaking temperatures for alkaline water-splitting was studied. The highly defective SNTO manifests properties similar to metallic Ni and favours H2 evolution through the hydrogen evolution reaction (HER) by adsorbing more H+ ions on active sites. In contrast, the ilmenite NTO favours O2 discharge. These results are explained based on the morphology of the NTO nanofibers. The mosaic structure which has higher porosity and greater SNTO content shows excellent HER performance. In contrast, the large bamboo structured NTO nanofibers which have lesser porosity and SNTO content cage the bigger (OH)ads ions at their catalytic sites to facilitate OER performance. 2019 © The Royal Society of Chemistry.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.