Simple Methods for the Preparation of Non-noble Metal Bulk-electrodes for Electrocatalytic Applications

J Vis Exp. 2017 Jun 21:(124):56087. doi: 10.3791/56087.

Abstract

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and composition of the material was characterized via powder X-ray diffraction (PXRD), Mössbauer spectroscopy (MB), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and energy dispersive X-ray spectroscopy (EDX). Two preparation methods of pentlandite bulk electrodes are presented. In the first approach a piece of synthetic pentlandite rock is directly contacted via a wire ferrule. The second approach utilizes pentlandite pellets, pressed from finely ground powder, which is immobilized in a Teflon casing. Both electrodes, whilst being prepared by an additive-free method, reveal high durability during electrocatalytic conversions in comparison to common drop-coating methods. We herein showcase the striking performance of such electrodes to accomplish the hydrogen evolution reaction (HER) and present a standardized method to evaluate the electrocatalytic performance by electrochemical and gas chromatographic methods. Furthermore, we report stability tests via potentiostatic methods at an overpotential of 0.6 V to explore the material limitations of the electrodes during electrolysis under industrial relevant conditions.

Publication types

  • Video-Audio Media

MeSH terms

  • Electrodes*
  • Electrolysis / instrumentation*
  • Electrolysis / methods*
  • Microscopy, Electron, Scanning / instrumentation*
  • Microscopy, Electron, Scanning / methods*