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    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.
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    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.
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    Synthesis and characterization of Ni-P-Ag composite coating as efficient electrocatalyst for alkaline hydrogen evolution reaction
    (Elsevier Ltd, 2016) Elias, L.; Hegde, A.C.
    The effect of addition of silver nanoparticle sol (SNS) into Ni-P plating bath was studied in terms of the variation in electrocatalytic behavior of the developed coatings in 1.0 M KOH. Ni-P-Ag composite coating was achieved through direct electrolysis by adding a known quantity of the conventionally prepared SNS into Ni-P bath. Ni-P-Ag coatings electrodeposited galvanostatically on copper under different conditions of the bath was used as electrode material for alkaline hydrogen evolution reaction (HER). The optimal concentration of the SNS required for maximum electrocatalytic activity towards HER was obtained by adding different volumes of SNS (from 0 to 50 mL L?1) into the bath. The HER efficiency of the test electrodes in 1.0 M KOH medium was examined using cyclic voltammetry (CV) and chronopotentiometry (CP) techniques. The kinetics of HER on the alloy and composite electrodes were established through Tafel polarization and electrochemical impedance spectroscopy (EIS) analyses. Energy dispersive spectroscopy (EDS) was used to confirm the incorporation of Ag nanoparticles into the Ni-P alloy matrix. The microstructure and morphology of the alloy and composite coatings were analyzed by Scanning Electron Microscopy (SEM). A significant improvement in the electrocatalytic property of nano-Ag derived composite coatings was found, and was attributed to the enhanced electroactive sites of Ag particles. Deposition conditions to maximize the electrocatalytic activity of Ni-P-Ag nanocomposite coatings in relation to traditional Ni-P alloy coatings was arrived, and results are discussed. © 2016
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    Electrodeposition and characterization of Ni-Mo alloy as an electrocatalyst for alkaline water electrolysis
    (Elsevier B.V., 2017) Shetty, S.; Mohamed, M.; Bhat, D.K.; Hegde, A.C.
    This work details the efficiency of Ni-Mo alloy as an electrode for water splitting application through electrodeposition method. Nano-crystalline Ni-Mo alloy coatings were deposited in the current density (c.d.) range of 1.0–4.0 A dm? 2 on a copper substrate, and were investigated for their deposit characters, and their electrocatalytic behaviours in 1.0 M KOH solution. The electrocatalytic behaviour of the coatings, in terms of their hydrogen evolution reaction (HER) and oxygen evolution reaction (OER), were evaluated by electrochemical methods, like cyclic voltammetry (CV) and chronopotentiometry (CP). Experimental results revealed that Ni-Mo alloy electrodeposited at 1.0 A dm? 2 (38.3 wt% Mo) and 4.0 A dm? 2 (33.2 wt% Mo) shows the highest electrocatalytic tendency for HER and OER, respectively. The corrosion behaviour of Ni-Mo alloy coated at 4.0 A dm? 2 is found to be the most corrosion resistant in the same alkaline medium, compared to other coatings. The highest electrocatalytic activity of Ni-Mo alloy deposit for both HER and OER, depending on deposition c.d. was attributed to their composition (in terms of Ni and Mo content), structure and surface morphology; supported by EDXA, XRD, SEM and AFM analyses. The experimental study demonstrated that Ni-Mo alloy coatings follow Volmer-Tafel type of mechanism for HER, testified by Tafel slope analyses. © 2017 Elsevier B.V.
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    Synthesis of effective electrocatalyst for water splitting application from simple Cu-Ni bath
    (Allerton Press Incorporation journals@allertonpress.com, 2017) Elias, L.; Banjan, R.U.; Hegde, A.C.
    Electrocatalytically active Cu-Ni alloy coatings have been developed from a simple electrolyte having only Cu+2 and Ni+2 ions, without the use of any additive. Electrocatalytic character of the coatings was tested for their hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) in 1.0 M KOH medium, alongside with their corrosion behaviours. Cyclic voltammetry and chronopotentio-metry study revealed that the deposition current density has a prominent role on the alkaline water splitting behaviour of the coatings, depending on their phase structure, composition and surface morphology. It was found that the c.d. has an inverse dependence on HER and OER. The Cu-Ni alloy coatings developed, respectively at 3.0 and 4.0 A dm–2, were found to be the best coatings for HER and OER, depending on the surface morphology. The electrocatalytic activity of Cu-Ni alloy coating for HER, deposited at 3.0 A dm–2 (optimal), was further improved through electrochemical dissolution of the as-deposited coating. The increase in the electrocatalytic activity for HER has been attributed to the enhancement in the exposed surface area of Ni active sites due to the leaching of Cu from the alloy matrices, evidenced by the energy-dispersive X-ray spectroscopy and scanning electron microscopy. The dependencies of HER and OER on to the surface of Cu-Ni alloy coatings were analysed in terms of deposition c.d. of the coatings, and the results are discussed. © 2017, Allerton Press, Inc.
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    RGO/ZnWO4/Fe3O4 nanocomposite as an efficient electrocatalyst for oxygen reduction reaction
    (Elsevier B.V., 2017) Mohamed, M.; Mutyala, S.; Mathiyarasu, J.; Bhat, D.K.
    Development of low cost, environmental friendly and noble metal free catalyst materials with excellent performance is essential for commercialization. In fact, this is the need of the day too. Herein, we report a facile microwave irradiation method for the synthesis of novel RGO/ZnWO4/Fe3O4 cathode catalysts for the oxygen reduction reaction (ORR) in alkaline medium. The structural and morphological features of synthesized materials are fully examined using transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM). The chemical composition and elemental analysis of the catalyst is investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy techniques. Efficiency of RGO/ZnWO4/Fe3O4 catalyst material for oxygen reduction reaction (ORR) in 0.1 M KOH is reported. The activity of catalyst is determined by linear sweep voltammogram (LSV) and rotating disk electrode (RDE) measurements in O2 saturated 0.1 M KOH electrolyte. RGO/ZnWO4/Fe3O4 catalyst exhibits higher ORR activity than RGO, ZnWO4, RGO/ZnWO4 and its electrocatalytic performance is comparable to Pt/C material and is superior to it in stability and methanol tolerance. Further, it is determined that process follows a direct four electron reaction pathway. These combined results strongly signpost that RGO/ZnWO4/Fe3O4 composite can function as an economic noble metal free ORR cathode catalyst for energy applications. © 2017 Elsevier B.V.
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    Porous nickel telluride nanostructures as bifunctional electrocatalyst towards hydrogen and oxygen evolution reaction
    (Elsevier Ltd, 2017) Bhat, K.S.; Barshilia, H.C.; Nagaraja, H.S.
    Electrochemical water splitting technology has attracted researchers for the development of next generation fuels. Herein, we report the synthesis of nanostructured porous hollow nickel telluride nanosheets and their use as bifunctional electrocatalyst towards hydrogen and oxygen evolution reaction, anticipating an enhanced performance owing to their 2D sheet like morphology, conductivity, porous nature providing larger catalytic surface for water splitting reaction. In this regard, nickel telluride nanostructures were synthesized via an anion-exchange-reaction between pre-synthesized nickel hydroxide hexagonal nanosheets and tellurium ions under hydrothermal conditions. The as-synthesized nanostructures were characterized for structural, morphological and compositional properties using X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, high resolution transmission electron microscopy and energy dispersive X-ray spectroscopy. Nickel telluride modified electrodes were tested as bifunctional electrocatalyst under acidic and alkaline conditions, through linear sweep voltammetry and constant current chronopotentiometry methods. The modified electrodes revealed an onset potential of ?422 mV and 87.4 mV dec?1 Tafel slope towards HER and overpotential of 679 mV and 151 mV dec?1 Tafel slope towards OER. The lower onset potentials are complimented with excellent electrocatalytic stability. © 2017 Hydrogen Energy Publications LLC
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    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.
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    Nickel selenide nanostructures as an electrocatalyst for hydrogen evolution reaction
    (Elsevier Ltd, 2018) Bhat, K.S.; Nagaraja, H.S.
    Electrochemical water splitting has gained momentum for the development of alternative energy sources. Herein, we report the synthesis of two different nickel selenide nanostructures of different morphology and composition employing hydrothermal method. NiSe2 nanosheets were obtained by the anion-exchange reaction of Ni(OH)2 with Se ions for 15 h. On the other hand, NiSe nanoflakes were synthesized by the direct selenization of nickel surface with the reaction time of 2 h. Tested as an electrocatalyst for hydrogen evolution reaction, NiSe2 nanosheets and NiSe nanoflakes can afford a geometric current density of 10 mA cm?2 at an overpotential of 198 mV and 217 mV respectively. The measured Tafel slope values of NiSe nanoflakes are 28.6 mV dec?1, which is three times lower as compared with NiSe2 nanosheets (72.1 mV dec?1). These results indicates the HER kinetics of NiSe nanoflakes are at par with the state-of-the-art Pt/C catalyst and also complimented with the short synthesis time of 2 h. Further, both nickel selenides exhibit ultra-long term stability for 30 h as evident from constant current chronopotentiometry and electrochemical impedance spectroscopy results. © 2018 Hydrogen Energy Publications LLC
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    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.