In this study, novel Co60Fe18Ti18B4 alloy powders have been synthesized with high compositional homogeneity using a high-energy ball milling technique. The structural, morphological and mechanical properties of the nanosized alloyed powders were examined using different analytical techniques, including scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectrometry and X-ray diffraction. According to the X-ray diffraction analysis for both Co powder and Co60Fe18Ti18B4 alloy powders, with increasing milling time, the content of Co-based (hcp) solid solution decreased and Co-based (fcc) solid solution increased. The mechanical properties of the material were also investigated by Vickers micro-hardness testing. The micro-hardness value of the Co60Fe18Ti18B4 alloy was found as 120.08 HV. After sintering (1 h– 1000 °C), the hardness improved remarkably (536.32 HV). Furthermore, results indicate that the synthesized Co-based alloy powder has both glassy and nanocrystalline phase forms.