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Carbon Nanofibers (CNF) are considered to be a promising catalyst support material due to their unique characteristics, excellent mechanical, electrical and structural properties, high surface area and nevertheless, good interaction with metallic catalyst particles. The possibility of preparing CNF decorated with platinum by an electrochemical method was tested, using a hexachloroplatinic bath solution. The experiments were carried out with the aid of a Potentiostat/Galvanostat Ivium Technologies Vertex, in a three – electrode cell. The aim of the present work was to determine the electrochemical surface area (ECSA) of the CNF-Pt catalysts in relation to the functionalization treatment of fibers, using an electrochemical method. ECSA for different functionalized CNF-Pt catalysts was determined by cyclic voltammetry in 0.5 M H2SO4 solution. The highest active surface of platinum was obtained for the samples with CNF functionalized by plasma treatment using 80 W for 1800 s. The obtained results correlate very well with the particles size and distribution of platinum, revealed by scanning electron microscopy (SEM) and the quantity of deposited platinum determined by thermo gravimetrical analysis (TGA) respectively. Cyclic voltammetry (CV) has been proven to be a suitable method for estimation of the ECSA of the electrocatalysts.
A systematic method for obtaining a novel electrode structure based on PtCoMn ternary alloy catalyst supported on graphitic carbon nanofibers (CNF) for hydrogen evolution reaction (HER) in acidic media is proposed. Ternary alloy nanoparticles (Co0.6Mn0.4 Pt), with a mean crystallite diameter under 10 nm, were electrodeposited onto a graphitic support material using a two-step pulsed deposition technique. Initially, a surface functionalisation of the carbon nanofibers is performed with the aid of oxygen plasma. Subsequently, a short galvanostatic pulse electrodeposition technique is applied. It has been demonstrated that, if pulsing current is employed, compositionally controlled PtCoMn catalysts can be achieved. Variations of metal concentration ratios in the electrolyte and main deposition parameters, such as current density and pulse shape, led to electrodes with relevant catalytic activity towards HER. The samples were further characterised using several physico-chemical methods to reveal their morphology, structure, chemical and electrochemical properties. X-ray diffraction confirms the PtCoMn alloy formation on the graphitic support and energy dispersive X-ray spectroscopy highlights the presence of the three metallic components from the alloy structure. The preliminary tests regarding the electrocatalytic activity of the developed electrodes display promising results compared to commercial Pt/C catalysts. The PtCoMn/CNF electrode exhibits a decrease in hydrogen evolution overpotential of about 250 mV at 40 mA cm−2 in acidic solution (0.5 M H2SO4) when compared to similar platinum based electrodes (Pt/CNF) and a Tafel slope of around 120 mV dec−1, indicating that HER takes place under the Volmer-Heyrovsky mechanism.