Publication date: 15th December 2025
Reliable electrocatalysis at industrially relevant current densities remains limited by poorly understood precatalyst reconstruction processes.1 Here, we integrate operando spectroscopies and theory to uncover how activation protocols dictate the structural and chemical evolution of NiFe precatalysts during the oxygen evolution reaction. We show that conventional cyclic voltammetry activation induces uncontrolled Fe oxidation, sulfur loss and irreversible degradation, leading to poor reproducibility and premature failure. Guided by thermodynamic and kinetic insights, we develop an operando-informed activation programming strategy based on controlled constant-potential oxidation, which selectively promotes Ni-centered reconstruction while suppressing Fe dissolution. Applied to a model NixFe1-xS2 platform, this programmed activation yields predictable transformation into stable Ni-rich oxyhydroxide phases, enabling durable operation in anion exchange membrane water electrolyzes at 1 A cm-2. The resulting cells exhibit a threefold improvement in reliability, achieving a low voltage degradation rate of 0.12 mV h-1 over 550 h. Beyond sulfides, the strategy generalizes across Fe-based oxides and layered hydroxides, establishing activation programming as a missing design dimension in catalyst development. This work bridges predictive modelling with experimentally validated reconstruction control, offering a pathway toward reliable high-current-density electrolysis and scalable green hydrogen production.
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