<p>Fe–Co–Al₂O₃ nanocomposite coatings were successfully synthesized on copper substrates using pulse electrodeposition. The results indicated that increasing the duty cycle led to the development of surface bumps and greater incorporation of Al₂O₃ nanoparticles into the coatings, with the 70% duty cycle resulting in the highest Al₂O₃ content. In contrast, at lower duty cycles, the coatings exhibited smoother, more uniform, and predominantly spherical surface morphologies. Transmission electron microscopy (TEM) revealed that the coatings had nanoscale and nanocrystalline structures. Furthermore, the microhardness of the coatings reached 580 HV at a 70% duty cycle. An increase in duty cycle also led to a reduction in the friction coefficient and wear rate. Overall, a 70% duty cycle was found to be optimal for the co-deposition of ceramic particles and the fabrication of Fe–Co–Al₂O₃ nanocomposite coatings with enhanced mechanical and tribological properties.</p>