Electrochemical conditioning via chronopotentiometry
(CP) and cyclic voltammetry (CV) is essential for the activation of
oxygen evolution reaction (OER) electrocatalysts. While many reports
have activated OER electrocatalysts using either CP or CV, the inherent
differences between these two electrochemical conditioning methods
for the activation of OER electrocatalytic materials have yet to be
explored. Here, we investigate the effects of CP and CV electrochemical
conditioning on a Ni-based OER precatalyst and substrate in Fe-purified
and Fe-unpurified KOH electrolytes by employing (i) Ni foil, (ii)
NiSe precatalyst films with different thicknesses on the fluorine-doped
tin oxide glass substrate, and (iii) NiSe precatalyst films on Ni
foil substrates. It was found that CV electrochemical conditioning
can result in a higher degree of in situ oxidation
and Fe incorporation for Ni-based precatalysts and substrates compared
to CP electrochemical conditioning. In turn, this brought about different
material properties (e.g., in situ oxidized layer thickness, composition, crystallinity, and morphology)
and electrochemical characteristics (e.g., active
surface area, electron transport limitation, and intrinsic activity)
of Ni-based electrocatalysts, thereby not only affecting their OER
activity but also complicating the interpretation of the origin of
OER activity. This study identifies the distinct effects of CP and
CV electrochemical conditioning on Ni-based OER electrocatalysts and
provides insight into the choice of the electrochemical conditioning
method to better investigate OER electrocatalysts.