Metal oxides are important functional
materials with a wide range of applications, especially in the field
of electrocatalysis. However, quick and accurate assessment of their
real electroactive surface area (ECSA), which is of paramount importance
for the evaluation of their performance, remains a challenging task.
Herein, we present a relatively simple strategy for an accurate in situ determination of the ECSA of commonly used metal
oxide catalysts, namely Ni-, Co-, Fe-, Pt-, and Ir-based oxides. Similar
to the well-established practice in electrocatalysis, the method is
based on the phenomenon of specific adsorption. It uses the fact that
at electrode potentials close to the onset of the oxygen evolution
reaction, specifically adsorbed reaction intermediates manifest themselves
through so called adsorption capacitance, which is unambiguously detectable
using electrochemical impedance spectroscopy. We determined and calibrated
these capacitances for common catalyst metal oxides using model thin
films. Therefore, with simple impedance measurements, experimentalists
can acquire the adsorption capacitance values and accurately estimate
the real electroactive surface area of the above-mentioned oxide materials,
including nanostructured electrocatalysts. Additionally, as illustrative
examples, we demonstrate the application of the method for the determination
of the ECSA of oxide catalyst nanoparticles.