Electrochemical dealloying as a post-treatment can greatly improve the catalytic activity of nanoparticles. To date, selecting suitable conditions to reach desired porosity, composition and catalytic activity is based on trial-and-error-attempts,...

Cobalt iron containing layered double hydroxides (LDHs) and spinels are promising catalysts for the electrochemical oxygen evolution reaction (OER). Towards development of better performing catalysts, the precise tuning of mesostructural features such as pore size is desirable, but often hard to achieve. Herein, a computer-controlled microemulsion-assisted co-precipitation (MACP) method at constant pH is established and compared to conventional co-precipitation. With MACP, the particle growth is limited and through variation of the constant pH during synthesis the pore size of the as-prepared catalysts is controlled, generating materials for the systematic investigation of confinement effects during OER. At a threshold pore size, overpotential increased significantly. Electrochemical impedance spectroscopy (EIS) indicated a change in OER mechanism, involving the oxygen release step. It is assumed that in smaller pores the critical radius for gas bubble formation is not met and therefore a smaller charge-transfer resistance is observed for medium frequencies.