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Journal of Analytical Methods in Chemistry
Volume 2016, Article ID 2030675, 16 pages
Research Article

Accurate Assessment of the Oxygen Reduction Electrocatalytic Activity of Mn/Polypyrrole Nanocomposites Based on Rotating Disk Electrode Measurements, Complemented with Multitechnique Structural Characterizations

1Dipartimento di Ingegneria dell’Innovazione, Università del Salento, Via Monteroni, 73100 Lecce, Italy
2Centro de Investigación, Innovación y Desarrollo de Materiales-CIDEMAT, Universidad de Antioquia UdeA, Calle 70 No. 52-21, Medellín, Colombia
3Institute for Microelectronics and Microsystems, IMM-CNR, Via Monteroni, 73100 Lecce, Italy

Received 21 August 2016; Revised 18 October 2016; Accepted 19 October 2016

Academic Editor: Chih-Ching Huang

Copyright © 2016 Patrizia Bocchetta et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.


This paper reports on the quantitative assessment of the oxygen reduction reaction (ORR) electrocatalytic activity of electrodeposited Mn/polypyrrole (PPy) nanocomposites for alkaline aqueous solutions, based on the Rotating Disk Electrode (RDE) method and accompanied by structural characterizations relevant to the establishment of structure-function relationships. The characterization of Mn/PPy films is addressed to the following: (i) morphology, as assessed by Field-Emission Scanning Electron Microscopy (FE-SEM) and Atomic Force Microscope (AFM); (ii) local electrical conductivity, as measured by Scanning Probe Microscopy (SPM); and (iii) molecular structure, accessed by Raman Spectroscopy; these data provide the background against which the electrocatalytic activity can be rationalised. For comparison, the properties of Mn/PPy are gauged against those of graphite, PPy, and polycrystalline-Pt (poly-Pt). Due to the literature lack of accepted protocols for precise catalytic activity measurement at poly-Pt electrode in alkaline solution using the RDE methodology, we have also worked on the obtainment of an intralaboratory benchmark by evidencing some of the time-consuming parameters which drastically affect the reliability and repeatability of the measurement.