Bocchetta Patrizia, Sánchez Carolina Ramírez, Taurino Antonietta, Bozzini Benedetto
Dipartimento di Ingegneria dell'Innovazione, Università del Salento, Via Monteroni, 73100 Lecce, Italy.
Centro de Investigación, Innovación y Desarrollo de Materiales-CIDEMAT, Universidad de Antioquia UdeA, Calle 70 No. 52-21, Medellín, Colombia.
J Anal Methods Chem. 2016;2016:2030675. doi: 10.1155/2016/2030675. Epub 2016 Nov 30.
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.
本文基于旋转圆盘电极（RDE）方法，报道了电沉积的锰/聚吡咯（PPy）纳米复合材料在碱性水溶液中氧还原反应（ORR）电催化活性的定量评估，并进行了与结构-功能关系建立相关的结构表征。锰/聚吡咯薄膜的表征涉及以下方面：（i）形态，通过场发射扫描电子显微镜（FE-SEM）和原子力显微镜（AFM）评估；（ii）局部电导率，通过扫描探针显微镜（SPM）测量；（iii）分子结构，通过拉曼光谱获取；这些数据为电催化活性的合理化提供了背景。为了进行比较，将锰/聚吡咯的性能与石墨、聚吡咯和多晶铂（poly-Pt）的性能进行了比较。由于文献中缺乏使用RDE方法在碱性溶液中多晶铂电极上进行精确催化活性测量的公认方案，我们还致力于通过证明一些严重影响测量可靠性和可重复性的耗时参数来获得实验室内部基准。
