Powder Catalyst Fixation for Post‐Electrolysis Structural Characterization of NiFe Layered Double Hydroxide Based Oxygen Evolution Reaction Electrocatalysts

Abstract Highly active electrocatalysts for the oxygen evolution (OER) reaction are in most cases powder nanomaterials, which undergo substantial changes upon applying the high potentials required for high‐current‐density oxygen evolution. Owing to the vigorous gas evolution, the durability under OER conditions is disappointingly low for most powder electrocatalysts as there are no strategies to securely fix powder catalysts onto electrode surfaces. Thus reliable studies of catalysts during or after the OER are often impaired. Herein, we propose the use of composites made from precursors of polybenzoxazines and organophilically modified NiFe layered double hydroxides (LDHs) to form a stable and highly conducting catalyst layer, which allows the study of the catalyst before and after electrocatalysis. Characterization of the material by XRD, SEM, and TEM before and after 100 h electrolysis in 5 m KOH at 60 °C and a current density of 200 mA cm −2 revealed previously not observed structural changes.