Electroless deposition of nickel and cobalt from alkaline baths as well as their codeposition with SiC particles were compared. It was found that despite similarity in properties of the metals their behavior in the electroless process was different. Maleic acid was used to stabilize plating baths, however the optimal concentration of the additive depended on the type of deposited metal. The electroless deposition characterized with low plating efficiency and it was higher for nickel than for cobalt. The composition as well as the morphology of Ni–P and Co–P deposits were also dissimilar. SiC particles inhibited the metal deposition, affected the plating potential, but did not alter the matrix composition. SiC entrapment was more preferential within the cobalt matrix than the nickel one. Some adsorption phenomena on SiC powder were also studied.