The aim of this work is to obtain and characterize the Niobium Carbide (NbC) by a suitable high energy milling technique using a SPEX Mill vibratory type and niobium and carbon (graphite) powders. Since this carbide is scarced in the national market and it’s necessary to apply this NbC as a reinforcement in two molybdenum high speed steels (AISI M2 and AISI M3:2) object of another work motivated this research. The powders were submitted to a high energy milling procedure for suitable times and conditions and then were characterized by means of Scanning Electronic Microscopy (SEM) and X-ray diffraction (DRX) techniques. The ball-to-powder weight ratio was 10:1. The analyzed samples showed that the high-energy milling is an alternative route of the NbC synthesis.