The presence of Ferrous ions is essential in Electro-Fenton (EF) and Photoelectro-Fenton (PEF) processes. To avoid the use of iron salts as precursors for the homogeneous Fenton process, iron was electrochemically deposited on a high surface area activated carbon (AC) material as previously reported by Santiago et al. for Pt-C particles. In this study, a novel rotating disk-slurry electrode (RoDSE) technique is employed to electrochemically prepare bulk iron/carbon (Fe/AC) material while avoiding a constant contact of the carbon support with an electrode surface. The electrochemically prepared Fe/AC was characterized, used to prepare an electrode and electrochemical experiments were performed to examine its performance as a cathode material for Electro- and Photoelectro-Fenton processes using a typical dye aqueous solution as a model effluent. The Fe/AC material exhibited a more complete (98%) and faster degradation performance, demonstrating that the use of the novel RoDSE technique is an effective method for preparing bulk quantities of activated carbon-supported iron for heterogeneous EF and PEF applications via an electrochemical route. The Author(s) 2015. Published by ECS. All rights reserved.