PtCu/CNT alloy electrocatalysts were prepared by microwave assisted polyol synthesis. The influence of preparation pH and the presence of polyvinylpyrrolidone (PVP) as stabilizer on catalysts nanostructure and activity towards electrocatalytic oxygen reduction was evaluated. The catalysts were alloyed at 400-600 degrees C for 6 h in reductive atmosphere, and characterized by TEM and XRD. The XRD patterns display a positive shift in 2 theta of the Pt 111 peak, which is a good evidence for Pt-Cu alloy formation. Alloy nanoparticles already form at temperatures as low as 400 degrees C. Highly agglomerated PtCu nanoparticles were obtained in the absence of PVP while PVP addition resulted in dispersed and uniform nanoparticles with a mean particle size of 3.7 nm. Such small particles are a result of the considerably low temperature used during the heat treatment/alloying step. However, while Pt is nearly completely deposited on the CNTs, only smaller fractions of Cu are found in the final catalyst. A high extent of agglomeration was also noticed when the pH during polyol synthesis was increased, which is attributed to Cu-hydroxides precipitation. Pt Cu core shell catalysts were obtained after voltammetric dealloying. Catalyst prepared at higher pH in the presence of PVP display the highest electrocatalytic activity. (C) 2014 Elsevier B.V. All rights reserved.