We realized the desired spheroidizing of NiCo₂O₄nanomaterials by laser irradiating NiCo₂O₄suspensions with different concentrations. The results reveal that the as-prepared samples are desired spheres with the maximal average size of 568 nm and the superior dispersity, which were obtained at the energy density of 0.30 J·pulse^-1·cm^-2and NiCo₂O₄suspension concentration of 0.2 mg·mL^-1. However, the phase segregation, which was induced by large amounts of solid redox of Co³⁺/Co²⁺and Ni³⁺/Ni²⁺, also appears in the laser-irradiation process.