Browsing by Author "Eugénio, S."
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- 3D nickel foams with controlled morphologies for hydrogen evolution reaction in highly alkaline mediaPublication . Siwek, K. I.; Eugénio, S.; Santos, Diogo; Moura E Silva, Teresa; MONTEMOR, FATIMAWater electrolysis is the cleanest method for hydrogen production, and can be 100% green when renewable energy is used as electricity source. When the hydrogen evolution reaction (HER) is carried out in alkaline media, nickel (Ni) is a low cost catalyst and an interesting alternative to platinum. Still, its performance has to be enhanced to meet the high efficiency of the nobler metals, an objective that requires further tailoring of the surface area and morphology of Ni-based electrode materials. Unlike commercially available porous Ni, these features can be easily controlled via electrodeposition, a one-step process, taking advantage of the dynamic hydrogen bubble template (DHBT). Generally, changes in surface porosity and morphology have been mainly achieved by altering the main parameters, such as the current density or the deposition time. However, very scarce work has been done on the role of supporting electrolyte (i.e., its concentration and composition) in tailoring the foam features and consequently their catalytic activity. Hence, this approach paves the way to optimum design of metallic foam structures that can be obtained only with modifications in the electrolytic bath. In this work, 3D Ni foams are obtained from different composition baths by galvanostatic electrodeposition in the hydrogen evolution regime on stainless steel current collectors. Their porosity and morphology are analysed by optical microscopy and SEM. The electrochemical performance is evaluated by cyclic voltammetry, while catalytic activity towards HER and materials' stability in 8 M KOH are tested using polarisation curves and chronoamperometry measurements, respectively. The recorded high currents and extended stability of the Ni foams with dendritic morphology demonstrate its outstanding performance, making it an attractive cathode material for HER in highly alkaline media. (C) 2018 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.
- Electrochemical performance of MnOx·center dot nH(2)O@Ni composite foam electrodes for energy storage in KOH mediaPublication . Siwek, Katarzyna; Eugénio, S.; Moura E Silva, Teresa; MONTEMOR, FATIMANanostructured porous MnO2, especially its hydrated amorphous and low crystalline form (MnO2·nH2O), has been one of the most promising material considered for charge storage applications, due to electrochemical similarities with RuO2 and its relative low cost. However, the intrinsic poor conductivity of MnO2 combined with the presence of structural water, which provides high ionic but low electronic conductivity, is a great hindrance for wider application. An effective approach to overcome this drawback involves the deposition of thin MnO2 layers on porous, high surface area metallic scaffolds. The present work addresses this route and provides novel insights thanks to the combination of MnOx·nH2O with custom-made Ni foams, fabricated via one-step electrodeposition using the dynamic hydrogen bubble template (DHBT). The porous Ni foams provide a scaffold with a 3D architecture with optimized pore size and surface. The composite electrode was fabricated by anodic deposition of MnOx·nH2O on the 3D Ni foams. The electrochemical behaviour was tested in 1 M KOH, since there are very few studies addressing the electrochemical behaviour of MnOx·nH2O in alkaline media for electrochemical supercapacitors applications. In addition, thermal treatment (150–250 °C) was performed to evaluate the effect of hydration on the material properties. The results revealed that the as-obtained composites are highly stable, displaying much higher specific capacitances with 73–90% (depending on the mass load) capacitance retention compared to their de-hydrated counterparts. The charge-discharge processes were found to be highly reversible throughout 5000 cycles, maintaining almost 100% columbic efficiency. In conclusion, the MnOx·nH2O@Ni composite electrodes showed a very stable pseudocapacitive behaviour and exceptional cycling performance in 1 M KOH, being therefore a promising alternative charge storage electrode for electrochemical supercapacitors.
- Electrodeposited reduced-graphene oxide/cobalt oxide electrodes for charge storage applicationsPublication . García-Gómez, A.; Eugénio, S.; Duarte, R.G.; Silva, Maria Teresa Oliveira de Moura e; Carmezim, M.J.; Montemor, M.F.In the present work, electrochemically reduced-graphene oxide/cobalt oxide composites for charge storage electrodes were prepared by a one-step pulsed electrodeposition route on stainless steel current collectors and after that submitted to a thermal treatment at 200 degrees C. A detailed physico-chemical characterization was performed by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and Raman spectroscopy. The electrochemical response of the composite electrodes was studied by cyclic voltammetry and charge-discharge curves and related to the morphological and phase composition changes induced by the thermal treatment. The results revealed that the composites were promising materials for charge storage electrodes for application in redox supercapacitors, attaining specific capacitances around 430 F g(-1) at 1 A g(-1) and presenting long-term cycling stability. (C) 2016 Elsevier B.V. All rights reserved.
- Electrodeposition and characterization of nickel–copper metallic foams for application as electrodes for supercapacitorsPublication . Eugénio, S.; Silva, Maria Teresa Oliveira de Moura e; Carmezim, M. J.; Duarte, R. G.; Montemor, M. F.Nickel-copper metallic foams were electrodeposited from an acidic electrolyte, using hydrogen bubble evolution as a dynamic template. Their morphology and chemical composition was studied by scanning electron microscopy and related to the deposition parameters (applied current density and deposition time). For high currents densities (above 1 A cm(-2)) the nickel-copper deposits have a three-dimensional foam-like morphology with randomly distributed nearly-circular pores whose walls present an open dendritic structure. The nickel-copper foams are crystalline and composed of pure nickel and a copper-rich phase containing nickel in solid solution. The electrochemical behaviour of the material was studied by cyclic voltammetry and chronopotentiometry (charge-discharge curves) aiming at its application as a positive electrode for supercapacitors. Cyclic voltammograms showed that the Ni-Cu foams have a pseudocapacitive behaviour. The specific capacitance was calculated from charge-discharge data and the best value (105 F g(-1) at 1 mA cm(-2)) was obtained for nickel-copper foams deposited at 1.8 A cm(-2) for 180 s. Cycling stability of these foams was also assessed and they present a 90 % capacitance retention after 10,000 cycles at 10 mA cm(-2).
- Electrodeposition and characterization of nikel-copper metallic foams for application as electrodes for supercapacitorsPublication . Eugénio, S.; Silva, Maria Teresa Oliveira de Moura e; Carmezim, M. J.; Duarte, R. G.; Montemor, M. F.Nickel-copper metallic foams were electrodeposited from an acidic electrolyte, using hydrogen bubble evolution as a dynamic template. Their morphology and chemical composition was studied by scanning electron microscopy and related to the deposition parameters (applied current density and deposition time). For high currents densities (above 1 A cm(-2)) the nickel-copper deposits have a three-dimensional foam-like morphology with randomly distributed nearly-circular pores whose walls present an open dendritic structure. The nickel-copper foams are crystalline and composed of pure nickel and a copper-rich phase containing nickel in solid solution. The electrochemical behaviour of the material was studied by cyclic voltammetry and chronopotentiometry (charge-discharge curves) aiming at its application as a positive electrode for supercapacitors. Cyclic voltammograms showed that the Ni-Cu foams have a pseudocapacitive behaviour. The specific capacitance was calculated from charge-discharge data and the best value (105 F g(-1) at 1 mA cm(-2)) was obtained for nickel-copper foams deposited at 1.8 A cm(-2) for 180 s. Cycling stability of these foams was also assessed and they present a 90 % capacitance retention after 10,000 cycles at 10 mA cm(-2).
- Electrodeposition: a versatile, efficient, binder-free and room temperature one-step process to produce MnO2 electrochemical capacitor electrodesPublication . Noce, R. Della; Eugénio, S.; Silva, T. M.; Carmezim, M. J.; Montemor, M. F.The use of room temperature cathodic electrodeposition to produce MnO2 electrochemical capacitor electrodes is demonstrated. By employing a permanganate-based bath, birnessite-type MnO2 electrodes are directly obtained with no further heat treatment. Moreover, a crystalline/amorphous structural transition is observed as the applied current density is increased up to 50 mA cm(-2).
- Fabrication of the three-dimensional dendritic Ni-Co films by electrodeposition on stainless steel substratesPublication . Silva, R. P.; Eugénio, S.; Silva, Maria Teresa Oliveira de Moura e; Carmezim, M. J.; Montemor, M. F.Co-deposition of nickel and cobalt was carried out on austenitic stainless steel (AISI 304) substrates by imposing a square waveform current in the cathodic region. The innovative procedure applied in this work allows creating a stable, fully developed, and open porous three-dimensional (3D) dendritic structure, which can be used as electrode for redox supercapacitors. This study investigates in detail the influence of the applied current density on the morphology, mass, and chemical composition of the deposited Ni-Co films and the resulting 3D porous network dendritic structure. The morphology and the physicochemical composition were studied by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and X-ray diffraction (W). The electrochemical behavior of the materials was evaluated by cyclic voltammetry (CV). The results highlight the mechanism involved in the coelectrodeposition process and how the lower limit current density tailors the film composition and morphology, as well as its electrochemical activity.
- Fabrication of Three-Dimensional Dendritic Ni-Co Films By Electrodeposition on Stainless Steel SubstratesPublication . Silva, R. P.; Eugénio, S.; Silva, Maria Teresa Oliveira de Moura e; Carmezim, M. J.; Montemor, M. F.Co-deposition of nickel and cobalt was carried out on austenitic stainless steel (AISI 304) substrates by imposing a square waveform current in the cathodic region. The innovative procedure applied in this work allows creating a stable, fully developed, and open porous three-dimensional (3D) dendritic structure, which can be used as electrode for redox supercapacitors. This study investigates in detail the influence of the applied current density on the morphology, mass, and chemical composition of the deposited Ni-Co films and the resulting 3D porous network dendritic structure. The morphology and the physicochemical composition were studied by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and X-ray diffraction (W). The electrochemical behavior of the materials was evaluated by cyclic voltammetry (CV). The results highlight the mechanism involved in the coelectrodeposition process and how the lower limit current density tailors the film composition and morphology, as well as its electrochemical activity.
- Hydrogen evolution on nanostructured Ni-Cu foamsPublication . Cardoso, D. S. P.; Eugénio, S.; Silva, Maria Teresa Oliveira de Moura e; Santos, D. M. F.; Sequeira, C. A. C.; Montemor, M. F.Three-dimensional (3D) nickel-copper (Ni-Cu) nanostructured foams were prepared by galvanostatic electrodeposition, on stainless steel substrates, using the dynamic hydrogen bubble template. These foams were tested as electrodes for the hydrogen evolution reaction (HER) in 8 M KOH solutions. Polarisation curves were obtained for the Ni-Cu foams and for a solid Ni electrode, in the 25-85 degrees C temperature range, and the main kinetic parameters were determined. It was observed that the 3D foams have higher catalytic activity than pure Ni. HER activation energies for the Ni-Cu foams were lower (34-36 kJ mol(-1)) than those calculated for the Ni electrode (62 kJ mol(-1)). The foams also presented high stability for HER, which makes them potentially attractive cathode materials for application in industrial alkaline electrolysers.