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Simple methods for the preparation of non-noble metal bulk-electrodes for electrocatalytic applications

: junge Puring, Kai; Piontek, Stefan; Smialkowski, Mathias; Burfeind, Jens; Kaluza, Stefan; Dötsch, Christian; Apfel, Ulf-Peter


Journal of visualized experiments : JoVE. Online resource (2017), Nr.124, Art. e56087; 6 S.
ISSN: 1940-087X
Fraunhofer UMSICHT Oberhausen ()
chemistry; inorganic chemistry; electrocatalysis; bulk electrode; iron nickel sulfide; hydrogen evolution reaction

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structureand composition of the material was characterized via powder X-ray diffraction (PXRD), Mössbauer spectroscopy (MB), scanning electronmicroscopy (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 over potential of 0.6 V to explore the material limitations of the electrodes during electrolysis under industrial relevant conditions.