Fe/N/C electrocatalysts for the oxygen reduction reaction (ORR) in polymer electrolyte membrane fuel cells (PEMFCs) have been synthesized from iron acetate ((FeAc)-Ac-II), 1,10-phenanthroline (phen), furfuryl alcohol (FA) and a thermally-decomposable metal-organic framework (MOF). The catalyst precursors have been prepared according to two main synthesis schemes. In the first one, a nitrogen-doped carbon was first synthesized from the MOF impregnated with FA, and this carbon was subsequently used as a microporous support for (FeAc)-Ac-II and phen. In the second approach, the FA-impregnated MOF was used as a support for (FeAc)-Ac-II and phen. The catalyst precursors prepared from these two approaches were subjected to a first pyrolysis in Ar and to a second pyrolysis in NH3. The effect of the pyrolysis temperature in Ar and heating rate were investigated. The as-prepared electrocatalysts were characterized by transmission electron microscopy, N-2 sorption analysis, as well as Mossbauer and X-ray absorption spectroscopies for the optimized catalysts. The electrochemical properties towards the ORR were investigated by rotating-disk electrode voltammetry and H-2-O-2 PEMFC tests. (C) 2013 Elsevier Ltd. All rights reserved.