The surfactant-free nanocrystalline NiCo2O4 nanoplates were synthesized using microwave irradiation method using metal chloride salts as precursors. Synthesized NiCo2O4nanoplateswere characterized using X-ray diffraction (XRD), fiel emission scanning electron microscope (FE-SEM), Energy dispersive spectrometer (EDS) for their structural and morphological and elemental analysis. Brunauer–Emmett-Teller (BET) surface area measurements show the surface area to be 11.60 m2/g and the crystallite size to be ∼14.74 nm. The optical studies show two Co3+ spin states contributions to band gap with values as 1.90 eV and 3.3 eV. The samples show high hydrophobicity, with good magnetic properties and conductivity.