Last modified: 2014-10-07
Abstract
For the first time, this study describes the sonoelectrochemical synthesis of Pt nanoparticles from solutions containing Pt salt, ionomer, solvent and water in the presence of ultrasound (20kHz,~100W.cm-2) using a specially designed/constructed Glassy Carbon (GC) electrode acting as a Vibrating Working Electrode (VWE) [Fig.1]. From early studies, it was found that Pt mean nanoparticle sizes could be produced in the range [11 - 15nm] in the absence of surfactants and solvents [1,2]. In this investigation, the syntheses of Pt nanoparticles were performed galvanostatically at (298±1)K, at various ultrasonic and current pulses using several time managements and at a high cathode efficiency. Physical characterisations by TEM, SEM, XRD and SAED showed that Pt mean grain sizes and cluster sizes of up to ~20nm and ~100nn were obtained respectively. Non-ultrasonicated (silent) but high-shear mixed catalyst inks made of Pt/C(Vulcan XC-72R)/Nafion®were prepared using the method described by Curnicket al. [3,4]. Electrochemical characterisation (Cyclic and RDE voltammetry) data of the as-prepared catalyst inks showed low ECSA values (<~35 m2.gPt-1). This finding was mainly attributed to: (i) the fairly ‘large’ Pt nanoparticle/cluster sizes, (ii) the ionomer acting as a ‘surfactant’ encapsulating the Pt nanoparticles thus preventing local electron transfer and (iii) poor dispersion of Pt nanoparticles/homogeneisation of the ink caused by the high-shear mixer (19,000rpm). However it was observed that the ionomer prevented Pt nanoparticles aggregation. It was suggested that the Nafion® content may play an important role on the activity of the Pt nanoparticles as previously observed [3,4]. It also possible that ultrasonication affects the composition and morphology of the electroanalyte/Pt nanoparticles/ionomer, mainly due to cavitation and sonolysis phenomena as recently shown by Pollet and Goh [5,6].
References
[1] V. Zin, B.G. Pollet, M. Dabala, Sonoelectrochemical (20 kHz) Production of Platinum Nanoparticles from Aqueous Solutions, Electrochem. Acta54 (2009) 7201-7206
[2] B.G. Pollet, The Use of Ultrasound for the Fabrication of Fuel Cell Materials, Int. J. Hydrogen Energy 35(21)(2010) 11986-12004
[3] O.J. Curnick, P.M. Mendes, B.G. Pollet, Enhanced Durability of a Pt/C Electrocatalyst Derived from Nafion®-Stabilised Colloidal Platinum Nanoparticles, Electrochem. Comm. 12(8) (2010) 1017-20
[4] O.J. Curnick, B.G. Pollet, P.M. Mendes, Nafion®-stabilised Pt/C Electrocatalysts with Efficient Catalyst Layer Ionomer Distribution for Proton Exchange Membrane Fuel Cells, RSC Advances 2 (22), (2012) 8368-8374
[5] B.G. Pollet, J.T.E Goh, The Importance of Ultrasonic Parameters in the Preparation of Fuel Cell Catalyst Inks, Electrochim. Acta, 128 (2014), 292–303
[6] B.G. Pollet, Electrocatalysis, 10.1007/s12678-014-0211-4