NiP (P > 10 wt.%) coatings are amorphous coatings whose structure can be transformed by heat treatment into a crystalline structure and hardened by precipitation of Ni3P. In this study, NiP coatings and composite ones with SiC nanoparticles were produced by electrodeposition, and their structural transformation by heat treatment was studied using differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The microhardness and the scratch and corrosion resistance of the coatings were evaluated and compared before and after different heat treatments. The results showed that in as-plated condition, the addition of SiC particles in the coatings did not modify the microstructure, microhardness, or electrochemical behavior. However, the SiC particles’ role was disclosed in combination with heat treatment. Composite coatings that were heat treated at 300◦C had higher microhardness and scratch resistance than the pure NiP one. In addition, composite coatings maintained their scratch resistance up to 400◦C, while in the case of the NiP ones, there was a reduction in scratch resistance by heating at 400◦C. It was also concluded that heating temperature has the main role in hardness and corrosion resistance of NiP and composite coatings, rather than heating time. The optimum heat-treatment protocol was found to be heating at 360◦C for 2 h, which resulted in a maximum microhardness of about 1500 HV0.02 for NiP and its composite coating without sacrificing the corrosion resistance.