Faculty Publications
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Item Electrolytic preparation of cyclic multilayer Zn-Ni alloy coating using switching cathode current densities(2010) Venkatakrishna, K.; Hegde, A.C.Cyclic multilayer alloy (CMA) coating of Zn-Ni was developed on mild steel using single bath technique, by proper manipulation of cathode current densities. The thickness and composition of the individual layers were altered precisely and conveniently by cyclic modulation of cathode current densities. Multilayer coatings, having sharp change in compositions were developed using square current pulses. Gelatin and sulphanilic acid (SA) acid were used as additives. Laminar deposits with different configurations were produced, and their corrosion behaviors were studied, in 5% NaCl solution by electrochemical methods. It was observed that the corrosion resistance of CMA coating increased progressively with number of layers (up to certain optimal numbers) and then decreased. Cyclic voltammetry study demonstrated the role of gelatin and SA in multilayer coating. The coating configuration has been optimized for the peak performance against corrosion. The substantial decrease of corrosion rate, in the case of multilayer coatings was attributed to the changed intrinsic electric properties, evidenced by Electrochemical Impedance Spectroscopy (EIS) study. The surface morphology and its roughness were examined by Atomic Force Microscopy (AFM). The surface and cross-sectional view of coatings were examined, using Scanning Electron Microscopy (SEM). X-ray photoelectron spectrum (XPS) study was carried out for surface analysis. The relative performance of pure Zn, monolithic and CMA coatings were compared and discussed. © 2010 Springer Science+Business Media B.V.Item Properties of ZnO:Bi thin films prepared by spray pyrolysis technique(Elsevier Ltd, 2013) Sadananda Kumar, N.; Bangera, K.V.; Anandan, C.; Shivakumar, G.K.Undoped and Bi doped zinc oxide thin films were deposited on glass substrate at 450 °C using spray pyrolysis technique. The X-ray diffraction studies shows that Bi doped ZnO films are polycrystalline hexagonal structure with a preferred orientation along (101) direction. Crystallites size of the films decreases with increasing doping concentration. Scanning electron microscope image shows change in the surface morphology. The composition of Zn, O and Bi elements in the undoped and Bi doped ZnO films were investigated by X-ray photoelectron spectroscopy. Bi doped ZnO thin films show a transparency nearly 75% in the visible region. The optical band gap of ZnO thin films reduces from 3.25 eV to 3.12 eV with an increase in Bi concentration from 0 to 5at.% respectively. Electrical conductivity of ZnO thin films increased from 0.156 to 6.02S/cm with increasing Bi dopant concentration from 0% to 5% respectively. © 2013 Elsevier B.V. All rights reserved.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 Reduced graphene oxide derived from used cell graphite and its green fabrication as an eco-friendly supercapacitor(Royal Society of Chemistry, 2014) Sudhakar, Y.N.; Muthu, M.; Bhat, D.; Senthil Kumar, S.Graphite extracted from a used primary cell was converted into reduced graphene oxide (rGO) using calcium carbonate together with rapid and local Joule heating by microwave irradiation. Electrodes were prepared by ultrasonically dispersing rGO in biodegradable poly(vinylpyrrolidone) (PVP) binder and coating this on recyclable poly(ethyleneterephthalate) (PET) sheet using a low cost screen printing technique. The use of the same polymer (PVP) as a binder, in addition to as the solid polymer electrolyte (SPE), enhances the compatibility and ionic conductivity of the hydrophobic rGO electrode in the supercapacitor system. Further, the phosphoric acid (H3PO4)-doped biodegradable SPE was screen printed for the first time on the rGO electrodes. Ionic conductivity and dielectric studies of the SPE were carried out at different temperatures and different dopant acid concentrations. The morphology, composition and structure of the graphene electrode components were characterized using Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) methods. Transmission electron microscopy (TEM) images showed a single layer or a few layers of rGO sheets and selected area electron diffraction showed the presence of slight defects. The fabricated environmentally friendly, industrially favorable and green supercapacitor showed a specific capacitance of 201 F g-1 and cyclic stability with 97% retention of the initial capacitance over 2000 cycles. Furthermore, the performance of this green supercapacitor is comparable to that of those fabricated using rGO synthesized from commercial graphite and in other literature reports. © 2014 The Royal Society of Chemistry.Item Novel one-pot green synthesis of graphene in aqueous medium under microwave irradiation using a regenerative catalyst and the study of its electrochemical properties(Royal Society of Chemistry, 2015) Subramanya, B.; Bhat, D.In this work we report an economic, eco-friendly, high yielding and facile one-pot method for the large scale synthesis of few layer graphene (FLG) nanosheets directly from graphite in aqueous medium using a regenerative catalyst, sodium tungstate. This method is fast and makes use of environmental friendly chemicals and microwave radiation. The as-synthesized FLG nanosheets are characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and Brunauer-Emmett-Teller (BET) surface area analysis. Raman analysis indicates that the as-synthesized graphene is bilayered with a smaller domain size of 3.9 nm which is responsible for a higher specific surface area of FLG nanosheets (1103.62 m2 g-1). Moreover, XPS analysis of FLG nanosheets shows a high C:O ratio (?9.6) which is the best among the graphene prepared from green chemicals. The electrochemical performance of as-synthesized FLG nanosheets is analysed by cyclic voltammetry (CV), chronopotentiometry and electrochemical impedance spectroscopy (EIS) in neat 1-ethyl-3-methylimidazolium tetrafluoroborate (EMIMBF4) electrolyte. The superior capacitive performance with large capacitance (219 F g-1), high energy density (83.56 W h kg-1) and excellent cyclability (3000 cycles) exhibited by these graphene nanosheets make them an excellent candidate for supercapacitor material. © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015.Item Novel Co-Ni-graphene composite electrodes for hydrogen production(Royal Society of Chemistry, 2015) Subramanya, B.; Ullal, Y.; Shenoy, S.U.; Bhat, D.; Hegde, A.C.Active, stable and cost-effective electrocatalysts are key to water splitting for hydrogen production through electrolysis. Herein, we report the facile preparation of highly porous Co-Ni-graphene (Co-Ni-G) composite electrodes by electrodeposition for electrocatalytic applications. The incorporation of graphene into the Co-Ni matrix enhances the catalyst's activity for the hydrogen evolution reaction (HER) in an alkaline solution. The best coating exhibits a maximum current density of -850 mA cm-2 at -1.6 V, which is approximately 4 times better than that of the binary Co-Ni alloy indicating higher activity for hydrogen production. The addition of graphene to an electrolyte bath results in a porous encapsulated bundle of alloy nano-particles within the graphene network which effectively increases the electrochemically active surface area. As indicated by XPS analysis results, on addition of graphene the Co(0) and Ni(0) content in the deposit increases and as a result both cobalt/cobalt oxide and nickel/nickel oxide sites are evenly distributed on the Co-Ni-G electrode surface which is responsible for increased HER activity. The Tafel slope analysis showed that the HER follows a Volmer-Tafel mechanism. The structure-property relationship of the Co-Ni-G composite coating has been discussed by interpreting field emission scanning electron microscopy (FESEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) analysis results. © The Royal Society of Chemistry 2015.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 Interparticle interactions and lacunarity of mechano-chemically activated fly ash(Elsevier, 2015) Patil, A.G.; Shanmugharaj, A.M.; Anandhan, S.A class F fly ash was subjected to high-energy ball milling-induced mechano-chemical activation aided by a surfactant. The resultant nanostructured fly ash was characterized by various techniques. X-ray fluorescence results showed that the amount of iron oxide was reduced from 4.39% to 2.75% after pre-treatment of fly ash by magnetic separation. Ethyl acetate as the milling medium, a ball to powder ratio of 12:1 and 2wt% of surfactant reduced the average particle size of fly ash to 329nm and led to a specific surface area of 8.73m2/g. The decrease in crystallite size of mechano-chemically activated fly ash was confirmed from a reduction in peak intensity with a broadened amorphous phase by X-ray diffraction studies. X-ray photoelectron spectroscopic characterization illustrated that peak area of major elements (O, Si and Al) increased after milling. Morphological and FTIR studies revealed that the smooth and inert surface of the fly ash was converted to a rough and more reactive one after mechano-chemical activation. The surface modification of fly ash with the surfactant was determined from FTIR spectroscopy. Also, a fractal approach was used to characterize the lacunarity of the agglomerates in the nanostructured fly ash. © 2014 Elsevier B.V.Item Novel Fe-Ni-Graphene composite electrode for hydrogen production(Elsevier Ltd, 2015) Badrayyana, S.; Bhat, D.K.; Shenoy, U.S.; Ullal, Y.; Hegde, A.We have developed a novel, efficient and economical composite electrode for hydrogen production. The electrode has been formed by embedding graphene in the Fe-Ni matrix via room temperature electrodeposition. The obtained active coatings have been tested for their efficiency and performance as electrode surfaces for hydrogen evolution reaction (HER) in 6 M KOH by cyclic voltammetry and chronopotentiometry techniques. The coating obtained at 60 mA cm-2 exhibited approximately 3 times higher activity for hydrogen production than that of binary Fe-Ni alloy. Addition of graphene to electrolyte bath resulted in porous 3D projections of nano-sized spheres of Fe-Ni on the surface of graphene, which effectively increased the electrochemically active surface area. XPS analysis results showed the equal distribution of both Ni metal and NiO active sites on the composite. The addition of graphene favoured the deposition of metallic nickel, which accelerated the rate determining proton discharge reaction. All these factors remarkably enhanced the HER activity of Fe-Ni-Graphene (Fe-Ni-G) composite electrode. The Tafel slope analysis showed that the HER follows Volmer-Tafel mechanism. The structure-property relationship of Fe-Ni-G coating has been discussed by interpreting field emission scanning electron microscopy (FESEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) analysis results. © 2015 Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.Item Novel RGO-ZnWO4-Fe3O4 nanocomposite as high performance visible light photocatalyst(Royal Society of Chemistry, 2016) Mohamed, M.M.J.; Shenoy, U.S.; Bhat, D.K.A novel RGO-ZnWO4-Fe3O4 nanocomposite is synthesized by a microwave irradiation method and its catalytic activity for the photo degradation of Methylene Blue (MB) is investigated. The prepared nanocomposites are characterized by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), high resolution transmission electron microscopy (HRTEM), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), Raman spectroscopy, photoluminescence spectroscopy (PL) and UV-visible spectroscopy. The visible light photocatalytic activities of the prepared nanocomposites are investigated using a MB dye solution. It is noteworthy that RGO-ZnWO4-Fe3O4 nanocomposites exhibited relatively high photocatalytic activity compared to ZnWO4-RGO and pure ZnWO4 on MB in aqueous solution. This enhanced rate is due to the ability of the graphene in the RGO-ZnWO4-Fe3O4 composite to support carrier exploitation efficiently by tolerating the photo excited electron-hole pairs and thus encouraging oxidative degradation of the pollutants. This work could be extended to other organic pollutants as well and could provide new insights into ternary nanocomposites as high performance photocatalysts and their application in waste water treatment. © 2016 The Royal Society of Chemistry.
