Nanoparticulate NiO and NiO/C composites with different carbon proportions have been prepared for anode application in lithium and sodium ion batteries. Structural characterization demonstrated the presence of metallic Ni in the composites. Morphological study revealed that the NiO and Ni nanoparticles were well dispersed in the matrix of amorphous carbon. The electrochemical study showed that the lithium ion batteries (LIBs) containing composites with carbon have promising electrochemical performances delivering specific discharge capacities of 550 mAh/g after operating for 100 cycles at 1C. These excellent results could be explained by the homogeneity of particle size and structure as well as the uniform distribution of NiO/Ni nanoparticles in the in situ generated amorphous carbon matrix. On the other hand, the sodium ion battery (NIB) with the NiO/C composite revealed a poor cycling stability. Post-mortem analyses revealed that this fact could be ascribed to the absence of a stable SEI or passivation layer upon cycling.