The present work deals with the formation of Ni-P/Ni-B duplex coatings by electroless plating and evaluation of their hardness and wear resistance. The duplex coatings were prepared with Ni-P as the inner layer. To analyze the structure of the coatings, XRD analysis was carried out. According to the results, Ni-P and Ni-B coatings are amorphous in their as-plated condition and after applying heat-treatment at 450 degrees C for 1 h, both Ni-P and Ni-B coatings crystallize and produce nickel, nickel phosphide and nickel borides in the coatings. To determine the surface morphology and cross-section characteristics of the coatings, SEM observations were carried out and concluded that duplex coatings are uniform and good coherent exists between the duplex layers and the coatings are also connected closely to the substrate. The hardness of electroless nickel duplex coatings increased with applying heat treatment and reached maximum value at coatings annealed at 400 degrees C. To analyze the tribological properties, pin-on-disc tests were carried out. The wear track patterns on the coatings and on Al2O3 balls were then examined by optical microscopy and EDS. The friction coefficient and wear rate of the coatings were lower than the substrate steel. Friction coefficient decreased from 0.43 to 0.36 and wear resistance decreased from 11.3 to 6.4 by applying heat treatment at 450 degrees C for 1 h to duplex coatings.