Polyacrylonitrile (PAN)-based carbon nanofiber Supported Fe/Co/Ni ternary alloy nanoparticles were prepared by using the electrospinning technique for potential fuel cell applications. The Solution Was prepared by adding pre-solved catalytic precursor into PAN/DMF Solution. The effect of PAN and catalyst precursor concentration on solution properties (viscosity and conductivity) and heat stabilization temperature has been investigated. Electrospun nanofibers were characterized by field emission scanning electron microscope, transmission electron microscope, energy dispersive spectrometer and X-ray diffractometer. It has been found that ternary nanoparticle size is in the range of 5-115 nm (average: 20 nm) and is a crystal alloy of Fe, Co and Ni. Also, TEM results demonstrate that in some regions metal nanoparticles tend to agglomerate into larger particles Mainly Clue to the non-uniform distribution Of nanoparticles in as-spun condition. PAN-derived carbon nanofiber mean diameter was measured as 200 nm by varying front 40 run to 420 nm. (C) 2009 Elsevier B.V. All rights reserved.