Abstract
In this study, we applied a two-step electrochemical anodization process to produce highly porous nanostructured nickel suboxides. We then annealed these materials in different environments: air, Ar, and Ar/H(2). Annealing in a reductive environment (Ar/H(2)) resulted in a Ni-NiO heterojunction with a high defect density, as confirmed by the Mott-Schottky analysis. Our results demonstrate that these defects and active sites significantly enhance the electrocatalytic activity for the oxygen evolution reaction (OER). Utilizing X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), and electrochemical analysis, we demonstrate that the heterojunction system containing Ni-NiO, formed through annealing in an Ar/H(2) atmosphere, acts as a highly efficient electrocatalyst for the OER. This catalyst achieves an impressively low overpotential of 293 mV at 10 mA cm(-2), a Tafel slope of 74 mV dec(-1), and exhibits outstanding stability, maintaining performance over 1000 cycles. Notably, our most optimized NiO (x) electrode outperforms the conventional reference RuO(2) electrode by a factor of 1.72. Our findings demonstrate the potential of binder-free Ni-NiO heterojunctions in developing high-performance electrocatalysts for alkaline electrolysis.